2-氯乙基3-氧代丁酸酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 6-bromo-2-pyridine aldehyde (1.542 g, 8.29 mmol), chloroethyl acetoacetate (1.388 g, 8.43 mmol) and methyl 3-aminocrotonate (948 mg, 8.29 mmol) in 12 ml of isopropanol was stirred under a nitrogen gas stream, at 40° C. for 9 hours and at room temperature for 13 hours. The reaction solvent was distilled off under reduced pressure, and the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (2:3)]. The crude product thus obtained was recrystallized from isopropyl ether-methanol to obtain 1.730 g (49% yield) of the above-captioned compound (m.p. 152° to 153°C.). at room temperature for 13 hours The reaction solvent was distilled off under reduced pressure the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (2:3)] The crude product thus obtained was recrystallized from isopropyl ether-methanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 6-Cyano-2-pyridine aldehyde (1.613 g, 12.2 mmol), chloroethyl acetoacetate (2.009 g, 12.2 mmol) and methyl 3-aminocrotonate (1.364 g, 12.2 mmol) were dissolved in 16 ml of isopropanol, and the solution was stirred at 35° to 40° C. under a nitrogen gas stream for 14 hours. The reaction solvent was distilled off under reduced pressure, and the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (5:6)]. The crude product thus obtained was recrystallized from isopropyl ether-methanol to obtain 1.546 g (34% yield) of the above-captioned compound. The reaction solvent was distilled off under reduced pressure the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (5:6)] The crude product thus obtained was recrystallized from isopropyl ether-methanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-nitrobenzaldehyde (4.536 g), 2-chloroethyl acetoacetate (4.94 g) and piperidine (110 mg) in benzene (18 ml) and acetic acid (360 mg) was refluxed for an hour under azeotropic dehydration. The reaction mixture was washed with water and dried. The solvent was distilled off to give an reddish oil of 2-chloroethyl 2-(2-nitrobenzylidene)acetoacetate, and thus obtained oil was treated with ethyl 3-amino-4,4-diethoxycrotonate (7.1 g) to give yellow granules of 2-chloroethyl 2-methyl-4-(2-nitrophenyl)-5-ethoxycarbonyl-6-diethoxymethyl-1,4-dihydropyridine-3-carboxylate, m.p. 82° to 84° C. (recrystallized from diisopropyl ether). was refluxed for an hour under azeotropic dehydration The reaction mixture was washed with water dried The solvent was distilled off

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-nitrobenzaldehyde (4.536 g), 2-chloroethyl acetoacetate (4.94 g) and piperidine (110 mg) in benzene (18 ml) and acetic acid (360 mg) was refluxed for an hour under azeotropic dehydration. The reaction mixture was washed with water and dried. The solvent was distilled off to give an reddish oil of 2-chloroethyl 2-(2-nitrobenzylidene)acetoacetate, and thus obtained oil was treated with ethyl 3-amino-4,4-diethoxycrotonate (7.1 g) to give yellow granules of 2-chloroethyl 2-methyl-4-(2-nitrophenyl)-5-ethoxycarbonyl-6-diethoxymethyl-1,4-dihydropyridine-3-carboxylate, m.p. 82° to 84° C. (recrystallized from diisopropyl ether). was refluxed for an hour under azeotropic dehydration The reaction mixture was washed with water dried The solvent was distilled off

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-nitrobenzaldehyde (4.536 g), 2-chloroethyl acetoacetate (4.94 g) and piperidine (110 mg) in benzene (18 ml) and acetic acid (360 mg) was refluxed for an hour under azeotropic dehydration. The reaction mixture was washed with water and dried. The solvent was distilled off to give an reddish oil of 2-chloroethyl 2-(2-nitrobenzylidene)acetoacetate, and thus obtained oil was treated with ethyl 3-amino-4,4-diethoxycrotonate (7.1 g) to give yellow granules of 2-chloroethyl 2-methyl-4-(2-nitrophenyl)- 5-ethoxycarbonyl-6-diethoxymethyl1,4 -dehydropyridine-3-carboxylate, m.p. 82° to 84° C. (recrystallized from diisopropyl ether). was refluxed for an hour under azeotropic dehydration The reaction mixture was washed with water dried The solvent was distilled off

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 6-bromo-2-pyridine aldehyde (1.542 g, 8.29 mmol), chloroethyl acetoacetate (1.388 g, 8.43 mmol) and methyl 3-aminocrotonate (948 mg, 8.29 mmol) in 12 ml of isopropanol was stirred under a nitrogen gas stream, at 40° C. for 9 hours and at room temperature for 13 hours. The reaction solvent was distilled off under reduced pressure, and the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (2:3)]. The crude product thus obtained was recrystallized from isopropyl ether-methanol to obtain 1.730 g (49% yield) of the above-captioned compound (m.p. 152° to 153°C.). at room temperature for 13 hours The reaction solvent was distilled off under reduced pressure the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (2:3)] The crude product thus obtained was recrystallized from isopropyl ether-methanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 6-Cyano-2-pyridine aldehyde (1.613 g, 12.2 mmol), chloroethyl acetoacetate (2.009 g, 12.2 mmol) and methyl 3-aminocrotonate (1.364 g, 12.2 mmol) were dissolved in 16 ml of isopropanol, and the solution was stirred at 35° to 40° C. under a nitrogen gas stream for 14 hours. The reaction solvent was distilled off under reduced pressure, and the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (5:6)]. The crude product thus obtained was recrystallized from isopropyl ether-methanol to obtain 1.546 g (34% yield) of the above-captioned compound. The reaction solvent was distilled off under reduced pressure the residue was purified by column chromatography [silica gel; ethyl acetate-n-hexane (5:6)] The crude product thus obtained was recrystallized from isopropyl ether-methanol

反应条件: temp:0.00; pressure:0.00; stir:

实验步骤: 投料: 往双口瓶加入2-氯乙基3-氧代丁酸酯（2.5eq）、醋酸铵（1.5eq）、甲醇（10V）和SM1（1g，6.62mmol）； 反应液加热至回流，保温6hr； LCMS显示反应完全； 反应液降至室温，再用冰浴降温1小时； 过滤，滤饼用甲醇淋洗； 滤饼干燥得黄色固体21g

实验步骤: 投料: 往双口瓶加入2-氯乙基3-氧代丁酸酯（2.5eq）、醋酸铵（1.5eq）、甲醇（10V）和SM1（1g，6.62mmol）； 反应液加热至回流，保温6hr； LCMS显示反应完全； 反应液降至室温； 过滤，滤饼用甲醇淋洗； 滤饼干燥得黄色固体0.8g

实验步骤: 09-20 12:23