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CAS No. : | 98437-23-1 | MDL No. : | MFCD01075674 |
Formula : | C8H7BO2S | Boiling Point : | - |
Linear Structure Formula : | (C6H4CHCS)B(OH)2 | InChI Key : | YNCYPMUJDDXIRH-UHFFFAOYSA-N |
M.W : | 178.02 | Pubchem ID : | 2359 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In 1,2-dimethoxyethane; water; at 90℃; for 15h; | A mixture of 5-bromo-7-iodo-/H-indazole (Preparation No.22a, 30.0 g, 92.9 mmol) and thianapthene-2-boronc acid (21.5 g, 120.7 mmol), DME (480 mL), water (48 mL), Na2CO3 (29.5 g, 279 mmol) and tetrakis triphenylphosphine palladium (0) (8.6 g, 7.43 mmol) was heated at about 90 0C in an oil bath under an atmosphere of nitrogen for about 15 hours. The solvent was removed under reduced pressure and the residue was suspended in a mixture of ethyl acetate (600 mL) and water (300 mL). The mixture was stirred for about 30 minutes and the resulting solid was collected by filtration and dried to yield 7-Benzo[b]ihiophen-2-yl-5-bromo-lH-indazole (21.4 g, 70%); (DMSO-^6, 400 MHz) δ 13.63 (s, IH), 8.24 (s, IH), 8.05-8.09 (m, 3H), 7.92 (d, IH), 7.65 (s, IH), 7.16 (m, 2H); RP-HPLC (Table 1, Method e) Rt = 2.69 min; m/v. (M-H)' 328.4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | palladium diacetate; In N,N-dimethyl-formamide; at 60 - 90℃; for 5 - 16h; | Example 44 Preparation of QR-0311[00400] Compound QR-031 1 was prepared by reactions depicted in Scheme 50 below.[00401] The following General Procedure H was used. <n="125"/>General Procedure H[00402] Arylbromide or aryliodide (1 mmol). boric acid ( 1.2 mmol) andPd(OAc)2 (0.05 mmol) in DMF (5 niL) were stirred under argon at 60-90 0C for 5-16 h. The mixture was then cooled to room temperature, ethyl acetate (50 mL) was added and the mixture washed with brine 3 times (50 mL). The organic layer wasdried with MgSO4 and concentrated. The residue was purified by flash columnchromatography.100403] General Procedure H was used to yield 259 (63% yield). 1H NMR(CDCl3): 2.38 (s, 3H). 7.30 (d, 2H. J=8.4). 7.37-7.41 (m, 2H), 7.55 (s, I H), 7.64 (d.1 H. J=8.6), 7.82-8-7.86 (m, 4H), 7.96 (s. 1 H), 8.14 (d. 1 H, .1=8.6). 8.31 (s, 1 H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 155℃; for 0.333333h;Microwave irradiation; | General procedure: To a mixture of compound 7a (1 mmol), the corresponding (het)arylboronic acid 10 (1.2 mmol), Pd(PPh3)4 (58 mg, 0.05 mmol) in degassed THF (3 mL), a solution of K2CO3 (346 mg, 2.5 mL) in water (4 mL) were added. The reaction mixture was microwave irradiated at 155 C (250 W) for 20 min, then solvent was removed in vacuo. Products were isolated by column chromatography (elution with ethyl acetate-hexane, 1 : 2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | With tetrakis(triphenylphosphine) palladium(0); potassium pivalate; In N,N-dimethyl acetamide; at 110℃; for 1.03333h;Inert atmosphere; | General procedure: In a flask of 20 ml, the diboronic acid and the 1,3-Dibromo-5-(2-ethylhexyl)-4H-thieno[3,4-c]pyrrole-4,6(5H)-dione are placed, subsequently 3 molar equivalents of potassium pivalate (PIVOK) are addedand finally 0.05 mol % of catalyst tetrakistriphenylphosphine Pd(PPh3)4 was added. The mixture wasplaced under nitrogen atmosphere, then 5 mL of dimethylacetamide (DMA) is added; the mixture wasstirred for 2 min and then heated up in the microwave at 110 C with a power of 100 W. After 1 h,the reaction was cooled down to 50 C and 50 mL of cold EtOH are added, a solid precipitate isobserved, which is filtered and washed first with 50 mL of EtOH and then with 50 mL of hexane.The solid was recovered and recrystallized using a mixture of ketone/EtOH 40:60. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In ethanol; water; toluene; for 12h;Inert atmosphere; Reflux; | A round bottom flask was charged with 13 g (41.8 mmol) of <strong>[689291-89-2]5-bromo-2-iodobenzaldehyde</strong>,Benzothiophene-2-boronic acid (7.8 g, 43.9 mmol),0.96 g (0.84 mmol) of tetrakistriphenylphosphine palladium, 17.3 g (125 mmol) of potassium carbonate, 130 ml of toluene, 52 ml of ethanol and 52 ml of water were put under a nitrogen atmosphere and refluxed for 12 hours. After completion of the reaction, the reaction product was separated into layers. The organic layer was concentrated under reduced pressure, and then separated by column chromatography to obtain 8.2 g of .10-a (Yield: 60%) |
60% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In ethanol; water; toluene; for 12h;Inert atmosphere; Reflux; | A round bottom flask was charged with 13 g (41.8 mmol) of <strong>[689291-89-2]5-bromo-2-iodobenzaldehyde</strong>,Benzothiophene-2-boronic acid (7.8 g, 43.9 mmol),0.96 g (0.84 mmol) of tetrakistriphenylphosphine palladium, 17.3 g (125 mmol) of potassium carbonate, 130 ml of toluene, 52 ml of ethanol,52 ml of water were added under nitrogen and refluxed for 12 hours.After completion of the reaction, the reaction product was separated, and the organic layer was concentrated under reduced pressure.Separation by column chromatography gave 8.2 g of intermediate 1-a. (Yield: 60%) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
16% | With dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; tris(dibenzylideneacetone)dipalladium(0) chloroform complex; potassium phosphate; In tetrahydrofuran; water; toluene; at 80℃; for 6h; | In the formula, Boc represents a tert-butoxycarbonyl group. The same applies to the following. ]To a solution of 2-benzothienylboronic acid (1.4 g) in toluene (20 mL) and water(0.779 g, 4.38 mmol) in THF (10 mL) was added tert-butyl (4-bromophenyl) carbamate (1.08 g, 3.97 mmol)Tris (dibenzylideneacetone) dipalladium (0) chloroform complex (Pd 2 (dba) 3 · CHCl 3; 29 mg, 0.028 mmol),2- (Dicyclohexylphosphino-2 ', 6'-dimethoxy-1,1'-biphenyl (S-Phos; 23 mg, 0.056 mmol),And K 3 PO 4 (1.39 g, 6.55 mmol) were added. The mixture was stirred at 80 C. for 6 hours,It was then extracted with toluene. After removing the solvent under reduced pressure,The mixture was subjected to silica gel column chromatography (2/1 hexane / CH 2 Cl 2), further purified by recrystallization from methanol,Compound 3-1 was obtained as colorless crystals (0.232 g, 0.713 mmol, 16%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89.6% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium phosphate tribasic trihydrate; In N,N-dimethyl-formamide; at 100℃; for 10h;Inert atmosphere; | General procedure: Toa degassed solution of <strong>[175205-81-9]2-bromo-4-(trifluoromethyl)pyridine</strong> (500 mg,2.21 mmol) and the corresponding boric acid (1.2 equiv) or boric acidester (SM-4, 1.2 equiv) in dry DMF (10 mL) were added Pd(dppf)Cl2(50 mg) and K3PO4*3H2O (1.18 g, 4.42 mmol). After 10 h heating at100 °C, the reaction mixture was cooled to room temperature, dilutedwith EtOAc (50 mL) and filtered through a pad of Celite. The filtratewas washed with H2O and brine. After the solvent was removed, theresidue was purified by column chromatography on silica gel, elutedwith EtOAc/hexanes (1:50, v/v) to give corresponding cyclometalatedligands |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
32.5% | With palladium bis[bis(diphenylphosphino)ferrocene] dichloride; potassium carbonate; In N,N-dimethyl-formamide; at 90℃; for 10h;Inert atmosphere; | General procedure: First, 1.0 g of 2-bromo-5-fluoropyridine (5.68 mmol),1.6 g of potassium carbonate (11.6 mmol)And 1.5 g of 2-boronic acid benzothiophene (8.43 mmol)Add to a 50 mL round bottom flask and then add 15 mL of 1,4-dioxane.Then 0.15 g of catalyst Pd(DPPF)2Cl2 was added.Pumping air immediately,The reaction was then heated to 90 ° C and stirred under nitrogen for 10 h.After the reaction was completed, the reaction solution was cooled to room temperature.Use thin plate chromatography to check for reaction,The resulting mixed solution was spin-dried using a rotary evaporator.The crude product was mixed with petroleum ether/ethyl acetate in a volume ratio of 100:1.The eluent is separated and purified by silica gel column chromatography.After drying in vacuum,0.46 g of the first intermediate 5-fluoro-2-pyridinebenzothiophene was obtained as a white powder.The yield was 35.4percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
20% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In methanol; toluene;Inert atmosphere; Reflux; | General procedure: <strong>[1458-01-1]Methyl 3,5-diamino-6-chloropyrazine-2-carboxylate</strong> 2 (1 eq.) was combined with K2CO3 (10 eq.), the appropriate (het)aryl boronic acid (1.5 eq.) and Pd(PPh3)4 (5 mol%) in a two-neck round bottom flask. The flask was connected to a condenser and purged with nitrogen. A 4:1 mixture of anhydrous toluene: MeOH (60 mL) was added via syringe and the reaction mixture was heated at reflux for 0.5-18 h. The mixture was allowed to cool to room temperature and filtered through Celite (10 x 3 cm, eluting with 3 x 20 mL EtOAc). The filtrate was evaporated to dryness and the residue purified by silica gel flash column chromatography using EtOAc/pet spirit. |
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