(R)-2-氨基丁酸甲酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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: An acetonitrile solution (15 ml) of 2-oximino-1-phenyl-1,3-butanedione (1.38 g, 7.22 mmoles) and methyl 2-aminobutyrate (0.85 ml, 7.22 mmol) was refluxed under nitrogen for 26.4 h. After concentrating the cooled reaction mixture, the residue was dissolved in 10 ml of ethanol and 20 ml of 10% aqueous sodium hydroxide. This mixture was refluxed 4.9 h, cooled, then extracted with ethyl acetate. Removal of the solvent in vacuo gave 0.65 g (42% yield) of 5-benzoyl-2-ethyl-4-methylimidazole and 5-acetyl-2-ethyl-4-phenylimidazole (86:14 respectively). After concentrating the cooled reaction mixture This mixture was refluxed 4.9 h cooled extracted with ethyl acetate Removal of the solvent in vacuo

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

实验步骤: To 4.99 g (0.039 moles) of 3-oximino-2,4-pentanedione dissolved in acetonitrile (40 ml) was added 4.59 ml (0.039 moles) of methyl 2-aminobutyrate. After stirring for two hours at room temperature, then at reflux for 2.5 h, the reaction mixture was cooled and treated with 15 ml of ethanol and 15 ml of 10% aqueous sodium hydroxide. The resulting mixture was refluxed for 3.8 h, cooled, then extracted with ethyl acetate. The combined organic extracts were dried over anhydrous sodium sulfate, then concentrated in vacuo to give 0.024 moles (62% yield) of 5-acetyl-2-ethyl-4-methylimidazole. at reflux for 2.5 h the reaction mixture was cooled The resulting mixture was refluxed for 3.8 h cooled extracted with ethyl acetate The combined organic extracts were dried over anhydrous sodium sulfate concentrated in vacuo

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

实验步骤: To 4.99 g (0.039 moles) of 3-oximino-2,4-pentanedione dissolved in acetonitrile (40 ml) was added 4.59 ml (0.039 moles) of methyl 2-aminobutyrate. After stirring for two hours at room temperature, then at reflux for 2.5 h, the reaction mixture was cooled and treated with 15 ml of ethanol and 15 ml of 10% aqueous sodium hydroxide. The resulting mixture was refluxed for 3.8 h, cooled, then extracted with ethyl acetate. The combined organic extracts were dried over anhydrous sodium sulfate, then concentrated in vacuo to give 0.024 moles (62% yield) of 5-acetyl-2-ethyl-4-methylimidazole. at reflux for 2.5 h the reaction mixture was cooled The resulting mixture was refluxed for 3.8 h cooled extracted with ethyl acetate The combined organic extracts were dried over anhydrous sodium sulfate concentrated in vacuo

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

实验步骤: 投料: 将2-氨基丁酸甲酯盐酸盐溶于DCM中，加入DIEA,，冰浴5℃下分批加入4-氯丁酰氯，有大量气体和热量产生，溶液由无色透明，变为浅黄色溶液，室温下搅拌3h； ，点板PE:EA=1-1,磷钼酸显色，反应完全； 后处理，用5%柠檬酸水溶液洗涤2次，饱和食盐水洗涤1次，有机相用无水硫酸钠干燥，过滤，旋蒸，得到黄色油状物

实验步骤: 投料: 将2-氨基丁酸甲酯盐酸盐溶于DCM中，加入DIEA,，冰浴5℃下分批加入4-氯丁酰氯，有大量气体和热量产生，溶液由无色透明，变为浅黄色溶液，室温下搅拌3h； ，点板PE:EA=1-1,磷钼酸显色，反应完全； 后处理，用5%柠檬酸水溶液洗涤2次，饱和食盐水洗涤1次，有机相用无水硫酸钠干燥，过滤，旋蒸，得到黄色油状物

实验步骤: 投料: 将2-氨基丁酸甲酯盐酸盐溶于DCM中，加入DIEA,，冰浴5℃下加入4-氯丁酰氯，有大量气体和热量产生，溶液由无色透明，变为浅黄色溶液，室温下搅拌过夜； 次日，点板PE:EA=1-1,磷钼酸显色，反应完全； 后处理，用5%柠檬酸水溶液洗涤2次，饱和食盐水洗涤1次，有机相用无水硫酸钠干燥，过滤，旋蒸，得到黄色油状物

实验步骤: 投料: 将原料溶于DCM中，0℃加入DIEA,4-氯丁酰氯，有大量白烟生成，0℃搅拌5min，后转室温搅拌1h； 点板原料反应完全，PE:EA=1:1,碘显； 后处理，用5%柠檬酸水溶液洗2次，饱和食盐水洗涤1次，有机相干燥过滤旋干，得到13.9g黄色油状物，核磁鉴定结构正确干净。