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Chemical Structure| 638-07-3 Chemical Structure| 638-07-3

Structure of 638-07-3

Chemical Structure| 638-07-3

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CAS No.: 638-07-3

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Product Details of [ 638-07-3 ]

CAS No. :638-07-3
Formula : C6H9ClO3
M.W : 164.59
SMILES Code : O=C(OCC)CC(CCl)=O
MDL No. :MFCD00000939
InChI Key :OHLRLMWUFVDREV-UHFFFAOYSA-N
Pubchem ID :69484

Safety of [ 638-07-3 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H301-H314
Precautionary Statements:P280-P301+P310-P305+P351+P338-P310
Class:8(6.1)
UN#:2922
Packing Group:Ⅱ

Computational Chemistry of [ 638-07-3 ] Show Less

Physicochemical Properties

Num. heavy atoms 10
Num. arom. heavy atoms 0
Fraction Csp3 0.67
Num. rotatable bonds 5
Num. H-bond acceptors 3.0
Num. H-bond donors 0.0
Molar Refractivity 37.24
TPSA ?

Topological Polar Surface Area: Calculated from
Ertl P. et al. 2000 J. Med. Chem.

43.37 ?2

Lipophilicity

Log Po/w (iLOGP)?

iLOGP: in-house physics-based method implemented from
Daina A et al. 2014 J. Chem. Inf. Model.

1.51
Log Po/w (XLOGP3)?

XLOGP3: Atomistic and knowledge-based method calculated by
XLOGP program, version 3.2.2, courtesy of CCBG, Shanghai Institute of Organic Chemistry

0.87
Log Po/w (WLOGP)?

WLOGP: Atomistic method implemented from
Wildman SA and Crippen GM. 1999 J. Chem. Inf. Model.

0.75
Log Po/w (MLOGP)?

MLOGP: Topological method implemented from
Moriguchi I. et al. 1992 Chem. Pharm. Bull.
Moriguchi I. et al. 1994 Chem. Pharm. Bull.
Lipinski PA. et al. 2001 Adv. Drug. Deliv. Rev.

0.64
Log Po/w (SILICOS-IT)?

SILICOS-IT: Hybrid fragmental/topological method calculated by
FILTER-IT program, version 1.0.2, courtesy of SILICOS-IT, http://www.silicos-it.com

1.35
Consensus Log Po/w?

Consensus Log Po/w: Average of all five predictions

1.02

Water Solubility

Log S (ESOL):?

ESOL: Topological method implemented from
Delaney JS. 2004 J. Chem. Inf. Model.

-1.08
Solubility 13.7 mg/ml ; 0.0835 mol/l
Class?

Solubility class: Log S scale
Insoluble < -10 < Poorly < -6 < Moderately < -4 < Soluble < -2 Very < 0 < Highly

Very soluble
Log S (Ali)?

Ali: Topological method implemented from
Ali J. et al. 2012 J. Chem. Inf. Model.

-1.36
Solubility 7.11 mg/ml ; 0.0432 mol/l
Class?

Solubility class: Log S scale
Insoluble < -10 < Poorly < -6 < Moderately < -4 < Soluble < -2 Very < 0 < Highly

Very soluble
Log S (SILICOS-IT)?

SILICOS-IT: Fragmental method calculated by
FILTER-IT program, version 1.0.2, courtesy of SILICOS-IT, http://www.silicos-it.com

-1.73
Solubility 3.09 mg/ml ; 0.0187 mol/l
Class?

Solubility class: Log S scale
Insoluble < -10 < Poorly < -6 < Moderately < -4 < Soluble < -2 Very < 0 < Highly

Soluble

Pharmacokinetics

GI absorption?

Gatrointestinal absorption: according to the white of the BOILED-Egg

 High
BBB permeant?

BBB permeation: according to the yolk of the BOILED-Egg

 Yes
P-gp substrate?

P-glycoprotein substrate: SVM model built on 1033 molecules (training set)
and tested on 415 molecules (test set)
10-fold CV: ACC=0.72 / AUC=0.77
External: ACC=0.88 / AUC=0.94

 No
CYP1A2 inhibitor?

Cytochrome P450 1A2 inhibitor: SVM model built on 9145 molecules (training set)
and tested on 3000 molecules (test set)
10-fold CV: ACC=0.83 / AUC=0.90
External: ACC=0.84 / AUC=0.91

 No
CYP2C19 inhibitor?

Cytochrome P450 2C19 inhibitor: SVM model built on 9272 molecules (training set)
and tested on 3000 molecules (test set)
10-fold CV: ACC=0.80 / AUC=0.86
External: ACC=0.80 / AUC=0.87

 No
CYP2C9 inhibitor?

Cytochrome P450 2C9 inhibitor: SVM model built on 5940 molecules (training set)
and tested on 2075 molecules (test set)
10-fold CV: ACC=0.78 / AUC=0.85
External: ACC=0.71 / AUC=0.81

 No
CYP2D6 inhibitor?

Cytochrome P450 2D6 inhibitor: SVM model built on 3664 molecules (training set)
and tested on 1068 molecules (test set)
10-fold CV: ACC=0.79 / AUC=0.85
External: ACC=0.81 / AUC=0.87

 No
CYP3A4 inhibitor?

Cytochrome P450 3A4 inhibitor: SVM model built on 7518 molecules (training set)
and tested on 2579 molecules (test set)
10-fold CV: ACC=0.77 / AUC=0.85
External: ACC=0.78 / AUC=0.86

 No
Log Kp (skin permeation)?

Skin permeation: QSPR model implemented from
Potts RO and Guy RH. 1992 Pharm. Res.

-6.69 cm/s

Druglikeness

Lipinski?

Lipinski (Pfizer) filter: implemented from
Lipinski CA. et al. 2001 Adv. Drug Deliv. Rev.
MW ≤ 500
MLOGP ≤ 4.15
N or O ≤ 10
NH or OH ≤ 5

 0.0
Ghose?

Ghose filter: implemented from
Ghose AK. et al. 1999 J. Comb. Chem.
160 ≤ MW ≤ 480
-0.4 ≤ WLOGP ≤ 5.6
40 ≤ MR ≤ 130
20 ≤ atoms ≤ 70

 None
Veber?

Veber (GSK) filter: implemented from
Veber DF. et al. 2002 J. Med. Chem.
Rotatable bonds ≤ 10
TPSA ≤ 140

 0.0
Egan?

Egan (Pharmacia) filter: implemented from
Egan WJ. et al. 2000 J. Med. Chem.
WLOGP ≤ 5.88
TPSA ≤ 131.6

 0.0
Muegge?

Muegge (Bayer) filter: implemented from
Muegge I. et al. 2001 J. Med. Chem.
200 ≤ MW ≤ 600
-2 ≤ XLOGP ≤ 5
TPSA ≤ 150
Num. rings ≤ 7
Num. carbon > 4
Num. heteroatoms > 1
Num. rotatable bonds ≤ 15
H-bond acc. ≤ 10
H-bond don. ≤ 5

 1.0
Bioavailability Score?

Abbott Bioavailability Score: Probability of F > 10% in rat
implemented from
Martin YC. 2005 J. Med. Chem.

0.55

Medicinal Chemistry

PAINS?

Pan Assay Interference Structures: implemented from
Baell JB. & Holloway GA. 2010 J. Med. Chem.

0.0 alert
Brenk?

Structural Alert: implemented from
Brenk R. et al. 2008 ChemMedChem

2.0 alert: heavy_metal
Leadlikeness?

Leadlikeness: implemented from
Teague SJ. 1999 Angew. Chem. Int. Ed.
250 ≤ MW ≤ 350
XLOGP ≤ 3.5
Num. rotatable bonds ≤ 7

 No; 1 violation:MW<1.0
Synthetic accessibility?

Synthetic accessibility score: from 1 (very easy) to 10 (very difficult)
based on 1024 fragmental contributions (FP2) modulated by size and complexity penaties,
trained on 12'782'590 molecules and tested on 40 external molecules (r2 = 0.94)

 1.88

Application In Synthesis of [ 638-07-3 ]

* 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 [ 638-07-3 ]

[ 638-07-3 ] Synthesis Path-Downstream   1~22

  • 1
  • [ 1824-81-3 ]
  • [ 638-07-3 ]
  • [ 87591-74-0 ]
YieldReaction ConditionsOperation in experiment
A mixture of 2-amino-6-methylpyridine (10.00 g, 92.47 mmol), ethyl 4-chloro- acetoacetate (16.24 mL, 120.2 mmol), and polyphosphoric acid (50.00 g) was stirred at 125 0C. After 5.5 h, the mixture was removed from the heat. To the cooled mixture was added ice-water (200 mL) and neutralized with 2 N NaOH (400 mL) to pH 6-7. The resulting precipitate was collected by filtration, washed with water (~ 400 mL), and dried to give 2-(chloromethyl)-6-methyl-4H-pyrido- [l,2-a]pyrimidin-4-one as a dark brown solid: 1H NMR (400 MHz, DMSO-d6) delta ppm 7.68 (1 H, dd, J=9.0, 7.0 Hz), 7.40 (1 H, dd, J=9.0, 0.8 Hz), 6.93 (1 H, d, J=6.7 Hz), 6.36 (1 H, s), 4.58 (2 H, s), 2.93 (3 H, s); Mass Spectrum (ESI) m/e = 208.9 (M + 1).
  • 2
  • [ 1128-56-9 ]
  • [ 638-07-3 ]
  • [ 88569-93-1 ]
  • 3
  • [ 30709-67-2 ]
  • [ 638-07-3 ]
  • [ 100003-88-1 ]
  • 4
  • [ 638-07-3 ]
  • [ 777-12-8 ]
  • ethyl-7-trifluoromethylimidazo<2,1-b>benzothiazole-2-acetate [ No CAS ]
  • 5
  • [ 2243-82-5 ]
  • [ 638-07-3 ]
  • [ 579525-03-4 ]
YieldReaction ConditionsOperation in experiment
13% at 160℃; for 1h; A mixture of 2-carbamoylnaphthalene (2.64 g, 15.4 mmol) and ethyl 4-chloroacetoacetate (2.06 g, 12.5 mmol) was stirred at 160°C for 1 hr. and then diluted with ethyl acetate (200 ml) at room temperature. The solution was washed with saturated sodium bicarbonate aqueous solution and brine in turn, and then dried. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate = 8 - 4) to give ethyl ester of [2-(2-naphthyl)oxazol-4-yl]acetic acid(459 mg, 13 percent) as yellow crystals. m.p.: 61.5 - 64 °C; IR (Nujol): 1737, 1591 cm-1; 1H-NMR (CDCl3): delta 1.31 (3H, t, J = 7.1 Hz), 3.73 (2H, d, J = 1.1 Hz), 4.24 (2H, q, J = 7.1 Hz), 7.49-7.57 (2H, m), 7.76 (1H, t, J = 1.1 Hz), 7.82-7.95 (3H, m), 8.11 (1H, dd, J = 1.7, 8.7 Hz), 8.58 (1H, br d, J = 1.1 Hz); APCI-MS m/z: 282 [M+H]+.
13% at 160℃; for 1h; 2) A mixture of 2-carbamoylnaphthalene (2.64 g, 15.4 mmol) and ethyl 4-chloroacetoacetate (2.06 g, 12.5 mmol)was stirred at 160° C. for 1 hr. and then diluted with ethyl acetate (200 ml) at room temperature. The solution waswashed with saturated sodium bicarbonate aqueous solution and brine in turn, and then dried. The solvent wasdistilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (nhexane/ethyl acetate=8-4) to give ethyl ester of [2- (2-naphthyl) oxazol-4-yl] acetic acid (459 mg, 13percent) as yellow crystals.m.p.: 61.5-64° C.; IR (Nujol): 1737, 1591 cm-1; 1H-NMR(CDCl3): delta1.31 (3H, t, J=7.1 Hz), 3.73 (2H, d, J=1.1 Hz),4.24 (2H, q, J=7.1 Hz), 7.49-7.57 (2H, m), 7.76 (1H, t, J=1.1 Hz), 7.82-7.95 (3H, m), 8.11 (1H, J=1.7, 8.7 Hz), 8.58(1H, br d, J=1.1 Hz); APCI-MS m/z: 282 [M+H]+
  • 6
  • [ 638-07-3 ]
  • [ 1903-91-9 ]
  • 6-(Chloromethyl)-4-hydroxy-2-(methoxymethyl)-pyrimidine [ No CAS ]
YieldReaction ConditionsOperation in experiment
With sodium methylate; In methanol; water; EXAMPLE 5 6-(Chloromethyl)-4-hydroxy-2-(methoxymethyl)-pyrimidine Sodium methylate (11.90 g, 0.22 mole) was added to a solution of <strong>[1903-91-9]methoxyacetamidine hydrochloride</strong> (12.45 g, 0.1 mole) and ethyl 4-chloroacetoacetate (16.50 g, 0.1 mole) in methanol (50 ml) at 5 to 10 C. with stirring. The resulting orange reaction mixture was stirred at 5 to 10 C. for 2 hours and then at 20 C. for 3 hours, and neutralized with conc. hydrochloric acid. The precipitate was filtered, and the filtrate was concentrated under reduced pressure to obtain a residue which was then dissolved in water (300 ml). The aqueous solution was extracted with chloroform, and the chloroform extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a crystalline residue. The residue was suspended in ether and then filtered to obtain 17.8 g of 6-(chloromethyl)-4-hydroxy-2-(methoxymethyl)pyrimidine as pale brown needle-like crystals (m.p. 124.0-125.5 C.).
  • 7
  • [ 62254-74-4 ]
  • [ 638-07-3 ]
  • 2-(5-Methylisoxazol-3-ylidene)-3-oxo-4-chlorobutyric acid ethyl ester [ No CAS ]
YieldReaction ConditionsOperation in experiment
EXAMPLE 69 2-(5-Methylisoxazol-3-ylidene)-3-oxo-4-chlorobutyric acid ethyl ester STR92 79.5 g of 5-methylisoxazole-3-aldehyde were reacted with 4-chloroacetoacetic acid ethyl ester as described in Example 24. A crude product, which was chromatographically pure, was obtained. This isomer ratio was 2:1. IR (film): 2950, 1720, 1590, 1420, 1255, 1225, 1020 cm-1. NMR (CDCl3): δ=7.64/7.61 [1] s, 6.21/6.08 [1] s, 4.47 [2] s, 4.40/4.32 [2] q, J=7 Hz, 2.43 [3] s, 1.32 [3] t, J=7 Hz ppm.
  • 8
  • [ 5319-77-7 ]
  • [ 638-07-3 ]
  • 7-chloromethyl-2-methylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidine-5-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide; In PPA; EXAMPLE 3 <strong>[5319-77-7]2-amino-5-methylthio-1,3,4-thiadiazole</strong> (9.4 g) was reacted with ethyl 4-chloro-acetoacetate (15.8 g) in polyphosphoric acid (50 g) under stirring at 100 C. for 1 hour. After cooling, dilution with ice water and neutralization with 35% NaOH, the precipitate was filtered and washed with water until neutral to give 7-chloromethyl-2-methylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidine-5-one, m.p. 168-169 C. (12.4 g), which was reacted with triphenylphosphine (14.4 g) in acetonitrile (250 ml) under stirring at reflux temperature for 24 hours.
  • 9
  • [ 638-07-3 ]
  • [ 621-63-6 ]
  • [ 225939-10-6 ]
YieldReaction ConditionsOperation in experiment
71.4% To a stirred suspension of 58,8 g 60 percent (1.47 mol) sodium hydride in 600 ml anhydrous tetrahydrofuran, a solution of 94 g (0.7 mol) 2,2-diethoxy-ethanol in 160 ml tetrahydrofuran was added dropwise, so that the temperature was kept below 40 'C. After completion of the addition, the reaction mixture was stirred for further 30 minutes. Then 115 g (0.7 mol) ethyl 4-chloroacetoacetate in 500 ml anhydrous tetrahydrofuran was added dropwise within 3 hours, so that the temperature was kept between 10 °C and 40 °C, preferentially at about 20 'C. The mixture was stirred overnight at room temperature. Then 90 ml ethanol was added dropwise, and the mixture was poured into 900 g of ice after which pH was adjusted to 6 with hydrochloric acid. The organic phase was separated and dried over MgSO4. The tetrahydrofuran was evaporated off and the product was separated from the oily layer in a separation funnel. Then the product was dissolved in toluene and purified by filtration through a short column of silica. The toluene was evaporated off, leaving the product as a light yellow oil. The product was purified by distillation in vacuo. yield: 130.9 g = 71.4 percent bp. = 112-114 'C at 0.2 mm Hg[] Elemental analysis: CalculatedC 54.9percentH 8.5percentFoundC 54.48percentH 8.7percentIR: 2986 cm-1; 1726 cm-1; 1748 cm-1; 1119 cm-1; 1067 cm-1 (Between KBr plates) NMR: 250 MHz 1H-NMR (CDCl3) (delta ppm): 4.646 (t, H, CH); 4.286 (s, 2H, CH2); 4.224 (s, 2H, CH2); 3,708 (q, 2H, CH2); 3.568 (q, 2H, CH2); 3.556 (d, 2H, CH2) ; 1.30 (t, 3H, CH3); 1.21 (m, 6H, CH3).
  • 10
  • [ 638-07-3 ]
  • [ 4922-98-9 ]
  • [ 1227417-79-9 ]
YieldReaction ConditionsOperation in experiment
67% With acetic acid; at 80℃; for 24h; Example 1; Part A; To the solution of 3-phenyl-1H-1 ,2,4-triazol-5-amine (0.8 g, 5 mmol) in acetic acid (6 mL) was added ethyl 4-chloro-3-oxobutanoate (0.75 mL, 5.5 mmol). The reaction mixture was stirred for 24 hours at 80 0C, and then cooled to room temperature. The reaction mixture was filtered. The precipitates were washed with ACN and dried to give compound 1-1 in a white powder (872 mg, 67percent yield). 1H NMR (400 MHz, CD3OD) delta 8.24-8.18 (m, 2H), 7.54-7.46 (m, 3H), 6.21 (s, 1H), 4.65 (s, 2H).; Example 6; Part A; To the solution of 3-phenyl-1 H-1 ,2,4-triazol-5-amine (0.8 g, 5 mmol) in acetic acid (6 ml_) was added ethyl 4-chloro-3-oxobutanoate (0.75 ml_, 5.5 mmol).The reaction mixture was stirred for 24 hours at 80 0C, and then cooled to room temperature. The reaction mixture was filtered. The precipitates were washed with ACN and dried to give compound 1-1 in a white powder (872 mg,67percent yield). 1H NMR (400 MHz, CD3OD) delta 8.24-8.18 (m, 2H), 7.54-7.46 (m,3H), 6.21 (s, 1 H), 4.65 (s, 2H).; Example 12; Part A; To the solution of 3-phenyl-1 H-1 ,2,4-triazol-5-amine (0.8 g, 5 mmol) in acetic acid (6 mL) was added ethyl 4-chloro-3-oxobutanoate (0.75 mL, 5.5 mmol). The reaction mixture was stirred for 24 hours at 80 0C, and then cooled to room temperature. The reaction mixture was filtered. The precipitates were washed with ACN and dried to give compound 1-1 in a white powder (872 mg, 67percent yield). 1H NMR (400 MHz, CD3OD) delta 8.24-8.18 (m, 2H), 7.54-7.46 (m, 3H), 6.21 (s, 1 H), 4.65 (s, 2H).
65.1% With acetic acid; at 80℃; <strong>[4922-98-9]3-phenyl-1H-1,2,4-triazole-5-amine</strong> (0.95 g, 5.93 mmol) obtained in Step 3-2 was dissolved in 15 mL of acetic acid and ethyl 4-chloroacetoacetate (1.07 g , 6.52 mmol), and the mixture was stirred at 80 ° C. overnight. After completion of the reaction, the precipitate was suction filtered to obtain 5-methylchloro-2-phenyl-[1,2,4]triazolo[1,5-a]pyrimidin-7(4H)-one (1.0 g, 86 mmol; yield 65.1percent)
  • 11
  • [ 75-15-0 ]
  • [ 2895-21-8 ]
  • [ 638-07-3 ]
  • [ 109-77-3 ]
  • [ 879033-77-9 ]
  • 12
  • [ 75-15-0 ]
  • [ 638-07-3 ]
  • [ 6092-47-3 ]
  • [ 109-77-3 ]
  • [ 879066-02-1 ]
  • 13
  • [ 75-15-0 ]
  • [ 638-07-3 ]
  • [ 6092-47-3 ]
  • [ 109-77-3 ]
  • [ 1189247-90-2 ]
  • 14
  • [ 75-15-0 ]
  • [ 638-07-3 ]
  • [ 19047-31-5 ]
  • [ 109-77-3 ]
  • [ 879033-82-6 ]
  • 15
  • [ 638-07-3 ]
  • [ 104-94-9 ]
  • [ 27143-07-3 ]
YieldReaction ConditionsOperation in experiment
EXAMPLES; Example 1; To a 30 gallon glass-lined reactor was charged water (26 L) and p-anisidine (8.5 kg; 68.1 moles). The reactor was inerted, and 20.1 kg 37percent HCl (3 eq.) were charged to the reactor followed by a line flush of 2 L purified water. The batch was heated to 40° C. and checked to ensure dissolution of p-anisidine (total time at 40° C. was 25 minutes). The batch was cooled to -2° C. and 40percent aqueous sodium nitrite (12.0 kg; 69.5 moles) was charged to the reactor while keeping the temperature at -2+/-3° C. The addition time for the aqueous sodium nitrite was 35 minutes. The sodium nitrite line was flushed with 2 L of purified water. The reaction mixture was sampled and analyzed for reaction completion. To the batch was added 3.0 kg of 11percent aqueous sulfamic acid via nitrogen pressure, keeping the reactor contents at -2+/-3° C. In a separate 100 gallon glass-lined reactor, 28 L of purified water was charged followed by 11.2 kg of solid sodium acetate. The reactor was inerted, and the batch was heated to 35° C. until the solid dissolved. The batch was cooled to 15° C. and 18 kg acetone was added to the reactor. To the reactor was added 12.4 kg ethyl-2-chloroacetoacetate by deadhead vacuum, followed by 2.1 kg of acetone to flush the addition line. The batch was cooled to -2+/-3° C. The contents of the above 30 gallon reactor were then transferred to the 100 gallon reactor keeping the batch in the 100 gallon reactor at -2+/-3° C. The transfer time was 45 minutes. The transfer line was flushed with 5.0 kg of acetone, and the batch was allowed to mix for one hour. To the reactor was charged 32.0 kg of acetone, and the batch was mixed for 15 minutes. The batch was allowed to settle for 30 minutes. To the reactor was charged 10.2 kg of acetone and the batch was mixed for 5 minutes. Agitation was stopped and the batch was allowed to settle for 30 minutes. The aqueous phase was discharged to a drum (140.2 kg; waste). To the reactor was charged 13.4 kg of methanol, controlling the reactor temperature to 0+/-3° C. The batch was held at 0+/-3° C. and sampled every hour until the reaction was complete. To the reactor was charged 75 L of purified water. The batch was heated to 5+/-5° C. and allowed to mix for 15 minutes. The batch was isolated using a portable centrifuge with a 5-7 micron polypropylene bag. The isolation lasted 10 minutes (109 kg of centrate). To the reactor was charged 26 L of purified water and 20.2 kg of methanol. The mixture was cooled to 5+/-3° C. and then discharged to the centrifuge to wash the cake. The wet cake (14.5 kg) was transferred to drying trays covered with FEP liners. The cake was dried at 40° C. for 80 hours to give 13.8 kg of the desired product.
  • 16
  • [ 638-07-3 ]
  • [ 32202-61-2 ]
  • C13H13NO2 [ No CAS ]
  • 17
  • [ 638-07-3 ]
  • [ 349-58-6 ]
  • [ 1353230-22-4 ]
  • 18
  • [ 638-07-3 ]
  • [ 349-58-6 ]
  • [ 1227692-71-8 ]
  • 19
  • [ 53051-97-1 ]
  • [ 638-07-3 ]
  • 10-(chloromethyl)-7-thia-1,9-diazatricyclo[6.4.0.02,6]dodeca-2(6),8,10-trien-12-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
4% With polyphosphoric acid; at 110℃; for 1h; A mixture of 4H,5H,6H-cyclopenta[d][l,3]thiazol-2-amine (2.00 g, 14.3 mmol) and ethyl 4- chloro-3-oxobutanoate (3.50 g, 21.3 mmol) in polyphosphoric acid (15 mL) was stirred for 1 h at 110 C. The reaction mixture cooled to room temperature, diluted with water (30 mL) and stirred for 1 h at 80 C. After cooling to room temperature, the reaction was quenched by water (200 mL), and the pH value ofthe solution was adjusted to pH 8-9 with potassium carbonate, extracted with dichloromethane (100 mL x 3), washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by chromatogtaphy with 20% ethyl acetate in petroleum ether to afford 10-(chloromethyl)-7-thia-l,9- diazatricyclo[6.4.0.0' [2,6]]dodeca-2(6),8,10-trien-12-one as a brown solid (150 mg, 4.0%). LCMS (ESI): M+H+ =241.1.
  • 20
  • [ 2362-63-2 ]
  • [ 638-07-3 ]
  • [ 54001-10-4 ]
YieldReaction ConditionsOperation in experiment
71% In ethanol; for 6h;Reflux; General procedure: To a solution of benzamide 11a-u (1 equiv) in THF (30mL) was added Lawesson’s reagent (0.6 equiv), and the mixture was heated to reflux for 4 hrs. The reaction mixture was concentrated invacuo,then diluted with ethyl acetate (30 ml), and washed with 1N NaHCO3 (3× 20 mL) and brine (2 × 20 mL). The organic layer was dried over anhydrous sodium sulfate,filtered and evaporated under reduced pressure. The crude product was purified by silica gel column chromatography using a mixture of dichloromethane/methanol(100:1, v/v) as eluent to afford a yellow solid product.A solution of the obtained solid 12a-u (1 equiv) and ethyl 2-chloroacetoacetate (1.2 equiv) in ethanol (25 ml) was heated to reflux for 6 h, then the mixture was allowed to stand at 0 C for 10 hrs, and a white needle crystal was precipitate out.The reaction mixture was filtered and the filter cake was washed with 10 mL of ethanol, dried in vacuum to give the desired product.
  • 21
  • [ 638-07-3 ]
  • [ 1192814-45-1 ]
  • 6,7-dichloro-2-(chloromethyl)-4H-pyrido[1,2-a]pyrimidin-4-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
31% With PPA; at 110℃; for 1h; Step 4: 6,7-Dichloro-2-(chloromethyl)-4H-pyrido[l,2-alpyrimidin-4-one: A mixture of <strong>[1192814-45-1]5,6-dichloropyridin-2-amine</strong> (4 g, 24.5 mmol), ethyl 4-chloro-3-oxobutanoate (8.1 g, 49.2 mmol) and PPA (21 g, 182 mmol) was stirred for 1 h at 110 C. The reaction was poured into water (50 ml) and the pH value of the solution was adjusted to 7 with sodium hydroxide (1 mol/L). The resulting solution was extracted with dichloromethane (3x200 ml) and then concentrated in vacuo. The residue was purified by chromatography with ethyl acetate/petroleum ether (1/3) to afford 6,7-dichloro-2-(chloromethyl)- 4H-pyrido[l,2-a]pyrimidin-4-one (2 g, 31%) as a brown solid. LCMS (ESI): M+H+ = 263.0. NMR (300 MHz, CDCI3) δ 7.58 (d, J = 4.8 Hz, 1H), 7.37 (d, J = 4.8 Hz, 1H), 6.57 (s, 1H), 4.45 (s, 2H).
  • 22
  • [ 638-07-3 ]
  • [ 2293-07-4 ]
  • C14H16N2O3S [ No CAS ]
YieldReaction ConditionsOperation in experiment
With poly(ethylene) glycol-600; at 20℃;Green chemistry; General procedure: mixture of 1 (10 mmol), 2 (10 mmol) and PEG-600(30 mL) was stirred at RT for 4-5 h. Then, salicylaldehyde(10 mM) and l-proline (25 mol %) was added into the samereaction vessel and the reaction mixture was stirred at RTfor a period of 2-3 h. After completion of the reaction, asshown by TLC analysis, the mixture was poured into icecoldwater (60 mL). The separated solid was filtered, washedwith water (2 × 30 mL) and air-dried at RT. The crude productwas recrystallized from suitable solvent to obtain pure 5.
 

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? Acyl Group Substitution ? Alkyl Halide Occurrence ? Baeyer-Villiger Oxidation ? Barbier Coupling Reaction ? Baylis-Hillman Reaction ? Bouveault-Blanc Reduction ? Bucherer-Bergs Reaction ? Catalytic Hydrogenation ? Clemmensen Reduction ? Complex Metal Hydride Reductions ? Corey-Bakshi-Shibata (CBS) Reduction ? Corey-Chaykovsky Reaction ? Ester Cleavage ? Fischer Indole Synthesis ? General Reactivity ? Grignard Reaction ? Heat of Combustion ? Henry Nitroaldol Reaction ? Hiyama Cross-Coupling Reaction ? Horner-Wadsworth-Emmons Reaction ? Hydride Reductions ? Kinetics of Alkyl Halides ? Kumada Cross-Coupling Reaction ? Lawesson's Reagent ? Leuckart-Wallach Reaction ? McMurry Coupling ? Meerwein-Ponndorf-Verley Reduction ? Passerini Reaction ? Paternò-Büchi Reaction ? Petasis Reaction ? Peterson Olefination ? Pictet-Spengler Tetrahydroisoquinoline Synthesis ? Preparation of Aldehydes and Ketones ? Preparation of Amines ? Prins Reaction ? Reactions of Aldehydes and Ketones ? Reactions of Alkyl Halides with Reducing Metals ? Reactions of Amines ? Reactions with Organometallic Reagents ? Reformatsky Reaction ? Robinson Annulation ? Schlosser Modification of the Wittig Reaction ? Schmidt Reaction ? Specialized Acylation Reagents-Carbodiimides and Related Reagents ? Specialized Acylation Reagents-Ketenes ? Stille Coupling ? Stobbe Condensation ? Substitution and Elimination Reactions of Alkyl Halides ? Suzuki Coupling ? Tebbe Olefination ? Ugi Reaction ? Wittig Reaction ? Wolff-Kishner Reduction

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