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[ CAS No. 1257220-47-5 ] {[proInfo.proName]}

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Chemical Structure| 1257220-47-5
Chemical Structure| 1257220-47-5
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Quality Control of [ 1257220-47-5 ]

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Product Details of [ 1257220-47-5 ]

CAS No. :1257220-47-5 MDL No. :MFCD26131198
Formula : C21H17N Boiling Point : No data available
Linear Structure Formula :- InChI Key :UAVZDBIKIOWDQF-UHFFFAOYSA-N
M.W : 283.37 Pubchem ID :66585204
Synonyms :

Calculated chemistry of [ 1257220-47-5 ]      Expand+

Physicochemical Properties

Num. heavy atoms : 22
Num. arom. heavy atoms : 19
Fraction Csp3 : 0.14
Num. rotatable bonds : 0
Num. H-bond acceptors : 0.0
Num. H-bond donors : 1.0
Molar Refractivity : 93.75
TPSA : 15.79 ?2

Pharmacokinetics

GI absorption : High
BBB permeant : No
P-gp substrate : Yes
CYP1A2 inhibitor : Yes
CYP2C19 inhibitor : Yes
CYP2C9 inhibitor : No
CYP2D6 inhibitor : No
CYP3A4 inhibitor : No
Log Kp (skin permeation) : -3.85 cm/s

Lipophilicity

Log Po/w (iLOGP) : 2.9
Log Po/w (XLOGP3) : 5.89
Log Po/w (WLOGP) : 5.63
Log Po/w (MLOGP) : 4.81
Log Po/w (SILICOS-IT) : 6.1
Consensus Log Po/w : 5.07

Druglikeness

Lipinski : 1.0
Ghose : None
Veber : 0.0
Egan : 0.0
Muegge : 2.0
Bioavailability Score : 0.55

Water Solubility

Log S (ESOL) : -5.95
Solubility : 0.00032 mg/ml ; 0.00000113 mol/l
Class : Moderately soluble
Log S (Ali) : -5.99
Solubility : 0.000287 mg/ml ; 0.00000101 mol/l
Class : Moderately soluble
Log S (SILICOS-IT) : -8.51
Solubility : 0.000000882 mg/ml ; 0.0000000031 mol/l
Class : Poorly soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 0.0 alert
Leadlikeness : 1.0
Synthetic accessibility : 2.47

Safety of [ 1257220-47-5 ]

Signal Word:Warning Class:
Precautionary Statements:P280-P305+P351+P338 UN#:
Hazard Statements:H302 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 1257220-47-5 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 1257220-47-5 ]

[ 1257220-47-5 ] Synthesis Path-Downstream   1~10

  • 1
  • [ 108-36-1 ]
  • [ 1257220-47-5 ]
  • [ 1369587-63-2 ]
YieldReaction ConditionsOperation in experiment
30% With sodium t-butanolate;tri-tert-butyl phosphine; palladium diacetate; In toluene; at 120℃; for 24h; Compound 6-2 (15g, 53mmol), 1,3-dibromobenzene (32mL, 265mmol), Pd(OAc)2 (1.2g, 5mmol), P(t-Bu)3 (30mL, 64mmol), NaOt-Bu (25g, 265mmol) and toluene 300mL were mixed and stirred at 120C for 24 hours. After termination of the reaction, the mixture was cooled to room temperature and extracted with EA 1.5L, and the obtained organic layer was washed with distilled water 400mL. Subsequently, the solvent was removed under reduced pressure and the obtained solid was washed with hexane, filtered and dried. Silcia gel column chromatography and recrystallization were performed, yielding Compound 6-3 (7g, 30%).
With tris-(dibenzylideneacetone)dipalladium(0); potassium tert-butylate; In water; toluene; at 110℃; for 24h;Inert atmosphere; In a 500 mL three-necked flask, 0.03 mol was added under nitrogen protection.Raw material B-4,0.03molM-dibromobenzene,250 mL of toluene was stirred and mixed, and then 0.09 mol of potassium t-butoxide was added.0.0015 mol Pd2(dba)3, heated to 110 C, refluxing for 24 hours;Naturally cooled to room temperature, filtered, and the filtrate was subjected to vacuum distillation (-0.09 MPa, 85 C).Passing through a neutral silica gel column to obtain intermediate C-2;
  • 2
  • [ 1300115-10-9 ]
  • [ 1257220-47-5 ]
YieldReaction ConditionsOperation in experiment
85% With tetrafluoroboric acid; palladium diacetate; potassium carbonate; In ethylenediamine; at 200℃; for 12h;Inert atmosphere; Under an argon atmosphere, a compound C8 (46.7 g, 14.6 mmol), Pd(OAc)2 (1.64 g, 7.32 mmol), HBF4 (3.62 g, 14.6 mmol), and K2CO3 (60.5 g, 438 mmol) and dimethylamide (50 ml). The reaction mixture was stirred at 200 C for 12 hours. After the reaction was terminated, the mixture was extracted with ethyl acetate. Drying with anhydrous MgSO4The organic layer obtained is filtered and the organic phase is concentrated.Compound obtained by column chromatography C9 (35.17g, 85%.
76% With palladium diacetate; 1,8-diazabicyclo[5.4.0]undec-7-ene; tricyclohexylphosphine; In N,N-dimethyl acetamide; at 170℃; for 8h; 2.1 Select 250ml three-necked flask, mechanical stirring rod, electric heating sleeve, weigh 12.7g HZ-1, 0.4g palladium acetate, 1.1g tricyclohexylphosphine, 11.8g DBU dissolved in 100ML DMAC, heating temperature to 170 C,Turn on the reaction;2.2 After 8 hours of reaction, the temperature was lowered to room temperature, and the reaction liquid was concentrated with an electric heating sleeve, and the product was dissolved in 200 ml.After washing with 200 ml of water for 5 times, the organic phase was dried to give a crude HZ-2.The crude product was pulverized with n-hexane to give 8.6 g, yield: 76%, HPLC: 99.9%.
73% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; caesium carbonate; In N,N-dimethyl acetamide; for 7h;Inert atmosphere; Reflux; Under nitrogen atmosphere, 25.0 g of N-(2-chlo- rophenyl)-9,9-dimethyl-fluorene-2-amine, 3.50 g of palladium(II) acetate, 7.70 g of di-tert-butyl(methyl)phosphoniumtetrafluoroborate, 127 g of cesium carbonate, and 600 mE of N,N-dimethylacetoamide were put into a flask and heated to reflux for seven hours while being stirred. Afier cooled down to the room temperature, the reaction solution was extracted with ethyl acetate. Afier an aqueous layer was removed, an organic layer was washed with a saturated saline solution. Afier dried with sodium sulfate, the organic layer was concentrated. The obtained residue was refined by silica-gel column chromatography and recrystallization, whereby 16.3 g (yield 73%) of a brown solid of an intermediate (F) was obtained.
53% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; In N,N-dimethyl acetamide; for 21h;Reflux; After mixing compound 1-1 (46 g, 143.8 mmol), Pd(OAc)2 (968 mg, 4.3 mmol), di-t-butyl(methyl)phosphoniumtetrafluoroborate (2 g, 4.31 mmol) and DMAc (200 mL), the reaction mixture was stirred for 21 hours under reflux. After terminating the reaction, the reaction mixture was filtered, and the filtered cake was washed with dichloromethane. The obtained organic layer was washed with purified water and dried with MgSO4, was concentrated under reduced pressure. And then, the crude oil was filtered through silica gel, and the remaining solution was concentrated under reduced pressure to obtain compound 1-2 (17 g, 53 %).
47% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; potassium carbonate; In N,N-dimethyl acetamide; at 200℃; for 12h; After mixing compound 1-1 (32 g, 0.1 mol), Pd(OAc)2 (1.1 g, 0.005 mol), di-t-butyl(methyl)phosphoniumtetrafluoroborate (2.48 g, 0.01 mol), K2CO3 (42 g, 0.30 mol) and DMA (550 mL), the reaction mixture was stirred for 12 hours at 200C. After terminating the reaction, the reaction mixture was extracted with EA. The obtained organic layer was dried with MgSO4, was filtered, was distillated under reduced pressure to remove the solvent, and was filtered through column to obtain compound 1-2 (14 g, 47 %).
47% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; potassium carbonate; at 200℃; for 12h; After mixing compound C-8-1 (32 g, 0.1 mol), Pd(OAc)2 (1.1 g, 0.005 mol), di-t-butylmethylphosphine·HBF4 (2.48 g, 0.01 mol), K2CO3 (42 g, 0.30 mol), and dimethyl amide (DMA) (550 mL), the mixture was stirred for 12 hours at 200C. After completing the reaction, the mixture was extracted with EA, and then the organic layer was dried with MgSO4. After filtering the obtained product, the solvent was removed under reduced pressure, and then the remaining product was separated with a column to obtain, white solid, compound C-8-2 (14 g, 47 %).
47% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; potassium carbonate; In N,N-dimethyl acetamide; at 200℃; for 12h; Compound 17-1 (32g, 0.1mol), Pd(OAc)2, (1.1g, 0.005mol), di-tert-butylmethylphosphine.HBF4 (2.48g, 0.01mol), K2CO3 (42g, 0.30mol), and DMA(550ml) were added, and then stirred at 200 for 12 hours. After completion of the reaction, extraction with ethyl acetate was performed on the resultant material, and then the organic layer is dried over MgSO4, followed by filtration. The solvent is removed under reduced pressure, followed by column chromatography, thereby obtaining Compound 17-2 (14g, 47 %).
43% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 5h;Reflux; In a flask was added Intermediate 18-3 (40g, 0,125mol), sodium carbonate (40g, 0.38mol), palladium acetate (0.5g, 2.2mmol), tricyclohexylphosphine tetrafluoroborate (1.6g, 4.4 mmol) and dimethylacetamide (0.5L), was heated at reflux for 5 hours, cooled, the solvent was evaporated under reduced partially removed, cooled, added to water, extracted with ethyl acetate, dried, purified by column to give the product 15g, yield 43%.
43% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 5h;Reflux; In a flask, intermediate 2-1 (40 g, 0.125 mol), sodium carbonate (40 g, 0.38 mol), palladium acetate (0.5 g,2.2 mmol), tricyclohexylphosphine tetrafluoroborate (1.6 g, 4.4 mmol) and dimethylacetamide (0.5 L) were heated at reflux for 5 hours, cooled, steamed to remove some of the solvent, cooled, and added to water. Ethyl acetate extraction, drying, and column purification gave 15 g of product in 43% yield.
43% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 5h;Reflux; In the flask,Intermediate 1-1 (40 g, 0.125 mol) was added,Sodium carbonate (40g, 0.38mol),Palladium acetate (0.5g, 2.2mmol),Tricyclohexylphosphine tetrafluoroborate (1.6 g, 4.4 mmol)And dimethylacetamide (0.5L),Heat reflux for 5 hours, cool,Steam distillation to remove some of the solvent,Cool, add water,Extract with ethyl acetate, dry,After column purification gives 15g product,Yield 43%.
42% With di-tert-butyl(methyl)phosphonium tetrafluoroborate salt; palladium diacetate; In N,N-dimethyl acetamide; for 24h;Reflux; To a solution of compound 9-1 (2.5 g, 7.8 mmol), di-tert-butylmethylphosphonium tetrafluoroborate ((t-Bu) 2PMeHBF4, 0.057 g, 0.23 mmol), Pd (OAc) 2 (0.05 g, 0.23 mmol) was dissolved in dimethylacetamide (DMAC, 80 ml) and refluxed with stirring for 24 hours. After cooling to room temperature, the mixture was concentrated under reduced pressure and extracted with methylene chloride and water. The extract was subjected to column chromatography using toluene: Hx to obtain Compound 9-2 (0.9 g, 42%).
36% With sodium carbonate;palladium diacetate; tricyclohexylphosphine tetrafluoroborate; In ISOPROPYLAMIDE; at 190℃; for 3h; Compound 6-1 (70g, 218mmol), Pd(OAc)2 (2.4g, 11mmol), PCy3HBF4 (8g, 22mmol), Na2CO3 (70g, 654mmol) and DMA 1.2L were mixed and stirred at 190C for 3 hours. After termination of the reaction, the mixture was extracted with EA 1L, and the obtained organic layer was washed with distilled water 200mL and dried with anhydrous MgSO4, and the organic solvent was removed under reduced pressure. The obtained solid was separated using silica gel column chromatography and recrystallization, yielding Compound 6-2 (22g, 36%).
36% With sodium carbonate; tricyclohexylphosphine tetrafluoroborate;palladium diacetate; In ISOPROPYLAMIDE; at 190℃; for 3h; Compound 12-1 (70g, 218mmol), Pd(OAc)2 (2.4g, 11mmol,) tricyclohexylphosphine tetrafluoroborate (8g, 22mmol), Na2CO3 (70g, 654mmol) and DMA (1.2L) were mixed, and stirred at 190C for 3 hours. After stirring, the reaction mixture was cooled to room temperature and extracted with EA. Column separation was conducted on the solid product, yielding Compound 12-2 (22g, 36%).
36% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; at 190℃; for 3h; After mixing compound 10-1 70 g (218 mmol), Pd(OAc)2 2.4 g (11 mmol), PCy3HBF4 8 g (22 mmol), Na2CO3 70 g (654 mmol), and dimethylacetamide (DMA) 1.2 L, the mixture was stirred at 190 C for 3 hours. After completing the reaction, the mixture was extracted with ethylacetate 1 L, the obtained organic layer was washed with distilled water 200 mL, and dried with anhydrous MgSO4. Then, the organic solvent was removed under reduced pressure. Then, the obtained solid was separated using silica gel column chromatography and recrystallization to obtain compound 10-2 22 g (36%).
36% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; at 190℃; for 3h; Compound 8-1 (70.0 g, 218.0 mmol), Pd(OAc)2 (2.4 g, 11.0 mmol), tricyclohexylphosphine tetrafluoroborate (PCy3HBF4) (8.0 g, 22.0 mmol), Na2CO3 (70.0 g, 654.0 mmol), and dimethylacetamide (DMA) (1.2 L) were mixed in a flask and stirred at 190C for 3 hrs. After completing the reaction, the mixture was extracted with EA (1.0 L), and the obtained organic layer was washed with distilled water (200.0 mL) and dried over anhydrous MgSO4. The organic solvent was removed under reduced pressure. After the separation of the obtained solid via column chromatography on silica gel and recrystallization, compound 8-2 (22.0 g, 36 %) was obtained.
36% With palladium diacetate; sodium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; at 190℃; for 3h; 70 g (218 mmol) of compound 10-1, 2.4 g (11 mmol) of Pd (OAc) 2, 8 g (22 mmol) PCy3HBF4, 70 g (654 mmol) of Na 2 CO 3 and 1.2 L of dimethylacetamide (DMA) were mixed and stirred at 190 C. for 3 hours. After the reaction, the mixture was extracted with 1 L of ethyl acetate, the organic layer was washed with 200 mL of distilled water, dried over anhydrous magnesium sulfate, and the organic solvent was removed under reduced pressure. The obtained solid was separated by silica gel column chromatography and recrystallization to give 22 g (36%) of compound 10-2.

  • 3
  • [ 1262866-93-2 ]
  • [ 1257220-47-5 ]
  • [ 1373227-56-5 ]
YieldReaction ConditionsOperation in experiment
70% Compound 12-2 (5g, 17.64mmol) and DMF (100mL) were mixed, and NaH (1.1g, 26.46mmol, 60% dispersion in mineral oil) was slowly added to the mixture. The mixture was stirred at room temperature for 30 minutes. After stirring, 4-(biphenyl-4-yl)-2-chloroquinazoline(5.6g, 17.64mmol) was slowly added to the mixture and stirred for 4 hours. After stirring, a solid product was obtained by adding distilled water (300mL) to the reaction mixture and stirring the reaction mixture for 30 minutes. Column separation was conducted on the solid product, yielding Compound 3 (6.9g, 70%). MS/EIMS: 563.69(found), 563.24(calculated)
  • 4
  • [ 1257220-47-5 ]
  • [ 1413615-86-7 ]
  • [ 1419576-90-1 ]
YieldReaction ConditionsOperation in experiment
36% After dissolving compound 1-2 (6.6 g, 18.6 mmol) in DMF (120 mL), NaH (813 mg, 20.3 mmol) was added at 0C, and was stirred for 10 minutes. Compound 1-3 (4.8 g, 16.9 mmol) was added to the reaction mixture, and was stirred for 19 hours. After terminating the reaction, MeOH was added to the reaction mixture. The obtained solid was filtered through silica gel, was recrystallized with DMF to obtain compound C-40 (4 g, 36 %).[99]MS/FAB found 603; calculated 602.73
  • 5
  • [ 1257220-47-5 ]
  • [ 1383627-88-0 ]
  • [ 1420118-21-3 ]
YieldReaction ConditionsOperation in experiment
50% After dissolving compound 1-2 (3.27 g, 11.5 mmol) in DMF (80 mL), NaH (507 mg, 12.7 mmol) was added at 0C, and was stirred for 10 minutes. Compound 2-1 (4.2 g, 12.1 mmol) was added to the reaction mixture, and was stirred for 7 hours. After terminating the reaction, MeOH was added to the reaction mixture. The obtained solid was filtered through silica gel, was recrystallized with DMF to obtain compound C-56 (3.4 g, 50 %).[115]MS/FAB found 590; calculated 589.73
  • 6
  • [ 1257220-47-5 ]
  • [ 1420067-46-4 ]
  • [ 1420120-27-9 ]
YieldReaction ConditionsOperation in experiment
48% After dissolving 60% NaH (1.0 g, 0.025 mol) in DMF (40 mL), the solution was stirred. After dissolving compound 1-2 (5.0 g, 0.017 mol) in DMF (40 mL), the solution was added to the above NaH solution, and was stirred for 1 hour. After dissolving compound 11-3 (7.2 g, 0.017 mol) in DMF (20 mL), and stirring, the mixed solution of compound 1-2 was added to the mixed solution of compound 11-3, and was stirred for 12 hours. The obtained yellow solid was filtered, was washed with MeOH, and was recrystallized to obtain compound C-41 (5 g, 48 %)[205]MS/FAB found 590; calculated 589.73
  • 7
  • [ 1257220-47-5 ]
  • [ 1383628-03-2 ]
  • [ 1420118-08-6 ]
YieldReaction ConditionsOperation in experiment
18% With sodium hydride; In N,N-dimethyl-formamide; mineral oil; at 20℃; for 12h; After dissolving compound 1-2 (4.5 g, 15.89 mmol) and compound 1-5 (7.3 g, 19.07 mmol) in dimethylformamide (DMF) (130 mL), 60% NaH in mineral oil (0.76 g, 19.07 mmol) was slowly added to the mixture, and was stirred for 12 hours at room temperature. After terminating the reaction, MeOH was added to the reaction mixture. The obtained solid was filtered through silica gel, was recrystallized with EA and DMF to obtain compound C-55 (1.8 g, 18 %). [108] MS/FAB found 630; calculated 629.79
  • 8
  • [ 1257220-47-5 ]
  • [ 914450-89-8 ]
  • [ 1346011-00-4 ]
YieldReaction ConditionsOperation in experiment
53% With potassium phosphate; tri-tert-butyl phosphine; palladium diacetate; In para-xylene; for 42h;Inert atmosphere; Reflux; [0155] 21.0 g (23.6 mmol) of compound IX, 53.4 g (188.4 mmol) of compound II and 203 g (960 mmol) of K3 PO4 are suspended in 3000 ml of p-xylene. 164 mg (0.73 mmol) of Pd(OAc)2 and 9.4 ml of a 1 M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 42 h. After cooling, the organic phase is separated off, washed three times with 400 ml of water and subsequently evaporated to dryness. The residue is washed with ethanol and recrystallised from toluene and finally dried under reduced pressure. The yield is 20.6 g (12.3 mmol), corresponding to 53% of theory.
  • 9
  • [ 1357150-72-1 ]
  • [ 1257220-47-5 ]
YieldReaction ConditionsOperation in experiment
85% With palladium diacetate; potassium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 12h;Reflux; 70 g (0.19 mol) of synthesized in Scheme 23, 1.4 g (0.004 mol) of tricyclohexylphosphinium tetrafluoroborate, 0.431 g (0.002 mol) of palladium acetate,53.1 g (0.384 mol) of potassium carbonate and 700 ml of N, N-dimethylacetamide were added and refluxed for 12 hours. After the completion of the reaction, the mixture was extracted and the organic layer was concentrated under reduced pressure and recrystallized with hexane to obtain 46.3 g (yield 85%).
85% With palladium diacetate; potassium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 12h;Reflux; In a 2 L round bottom flask, 70 g (0.19 mol) of the compound represented by formula 4-c obtained from Scheme 9, 1.4 g (0.004 mol) of tricyclohexylphosphinium tetrafluoroborate, 0.431 g (0.002 mol) of palladium acetate,Potassium carbonate 53.1 g (0.384 mol) and 700 mL of N,N-dimethylacetamide were added and refluxed for 12 hours. After completion of the reaction, extraction, the organic layer was concentrated under reduced pressure, recrystallized with hexane, and dried to obtain 46.3g (85%).
85% With palladium diacetate; potassium carbonate; tricyclohexylphosphine tetrafluoroborate; In N,N-dimethyl acetamide; for 12h;Reflux; In a 2L round bottom flask, 70 g (0.19 mol) of the compound of formula 5-b obtained from Scheme 9, 1.4 g (0.004 mol) of tricyclohexylphosphinium tetrafluoroborate, 0.431 g (0.002 mol) of palladium acetate, and potassium carbonate 53.1 g (0.384 mol) and 700 mL of N,N-dimethylacetamide were added and refluxed for 12 hours. After the reaction was completed, the organic layer was concentrated under reduced pressure, recrystallized from hexane and dried to obtain 46.3 g (85%) of .10-c
55.2% With tetrakis(triphenylphosphine) palladium(0); potassium acetate; In N,N-dimethyl-formamide; at 100℃; for 11h;Inert atmosphere; Example 1 Synthesis of 12,12-dimethyl-10-phenyl-7-(9-phenyl-9H-carbazol-3-yl)-10,12-dihydroindeno[2,1-b]carbazole (Compound 5) N-(9,9-dimethyl-9H-fluorene-2-yl)-2-bromo-aniline (18.5 g), potassium acetate (6.98 g), and DMF (95 ml) were added to a nitrogen-substituted reaction vessel and aerated with nitrogen gas for 1 hour. The mixture was heated after adding tetrakis(triphenylphosphine)palladium (1.18 g) and stirred at 100C for 11 hours. After the mixture was cooled to a room temperature, the reaction liquid was added to water (300 ml) and extraction was performed with toluene (300 ml). An organic layer obtained was washed with water (200 ml) twice, dehydrated with anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain a crude product. The crude product was purified by column chromatography (carrier: silica gel; eluent: toluene/n-hexane) to obtain a pale yellow powder of 12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole (7.9 g; yield 55.2%).
55.2% With tetrakis(triphenylphosphine) palladium(0); potassium acetate; In N,N-dimethyl-formamide; at 100℃; for 12h;Inert atmosphere; In the reaction vessel replaced by nitrogen, add:N-(9,9-dimethyl-9H-fluorene-2-yl)-2-bromoaniline18.5g,Potassium acetate 6.98g, DMF: 95ml, nitrogen aeration for 1 hour.Add four (triphenylphosphine) palladium1.18g and heated, and stirred at 100C for 11 hours. The reaction solution was cooled to room temperature, and 300ml of water was poured into it,300 ml of toluene was used for extraction.The organic layer was washed twice with 200 ml of water, dehydrated with anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain a crude product.Chromatography Analyzer for Crude Material Utilization Column(Carrier: silica gel, eluent: toluene/n-hexane) refined to obtain12,12-Dimethyl-10,12-indan[2,1-b]carbazoleYellow powder7.9g (yield 55.2%).

  • 10
  • [ 92-66-0 ]
  • [ 1257220-47-5 ]
  • [ 1257248-17-1 ]
YieldReaction ConditionsOperation in experiment
88.1% With 3,5-ditertbutyl salicylic acid; copper; potassium carbonate; sodium hydrogensulfite; at 190℃; for 26h;Inert atmosphere; Example 6 Synthesis of 10-(biphenyl-4-yl)-12,12-dimethyl-7-(9-phenyl-9H-carbazol-3-yl)-10,12-dihydroindeno[2,1-b]carbazole (Compound 122) <strong>[1257220-47-5]12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole</strong> synthesized in Example 1 (35.5 g), 4-bromobiphenyl (35.0 g), sodium bisulfite (6.0 g), a copper powder (2.4 g), 3,5-di(tert-butyl)salicylic acid (9.4 g), potassium carbonate (31.2 g), and dodecylbenzene (52 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 190C for 26 hours. After cooled to 120C, the mixture was stirred after adding toluene (35 ml), and a crude product was collected by filtration. After adding toluene (1.6 L) to the crude product, the crude product was heated and extracted at 110C. After cooled to a room temperature, the crude product was concentrated under reduced pressure. The product was crystallized with methanol (120 ml) to obtain a white powder of 10-(biphenyl-4-yl)-<strong>[1257220-47-5]12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole</strong> (48.5 g; yield 88.1%). The resulting 10-(biphenyl-4-yl)-<strong>[1257220-47-5]12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole</strong> (42.5 g) and DMF (2.5 L) were added to a reaction vessel, and the mixture was heated up to 70C and dissolved.
88.1% With 3,5-ditertbutyl salicylic acid; copper; potassium carbonate; sodium hydrogensulfite; at 190℃; for 26h;Inert atmosphere; In the reaction vessel replaced by nitrogen, add:35.5 g of 12,12-dimethyl-10,12-indan[2,1-b]carbazole synthesized in Example 1,4-bromobiphenyl 35.0g,6.0g of sodium bisulfite, 2.4g of copper powder, 9.4g of 3,5-bis(tert-butyl)salicylic acid,31.2 g of potassium carbonate and 52 ml of dodecylbenzene were heated and stirred at 190C for 26 hours. It was cooled to 120C, 35 ml of toluene was added and stirred, and the crude product was collected by filtration.1.6L of toluene was added to the crude product and heated, and after extraction was performed at 110C,Cool to room temperature and concentrate under reduced pressure. Use 120ml methanol for crystallization,Obtain 10-(biphenyl-4-yl)-12,12-dimethyl-10,12-indane [2,1-b]Carbazole48.5g of white powder (yield 88.1%).
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