HRID1912448

反应详情

EQUATION

反应方程式

HRID 1912448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

rac-2-Amino-2-(3-bromo-phenyl)-propionitrile (20 g, 88.9 mmol) was dissolved in HCl/MeOH (500 mL) and the mixture was refluxed for 4 days. After cooling to room temperature, AcOEt (100 mL) and water (100 mL) were added and the mixture was extracted with AcOEt (2×100 mL). The combined aqueous layers were basified with aqueous ammonia solution until pH 8 and extracted with AcOEt (5×100 mL). The combined organic layers were dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield rac-2-amino-2-(3-bromo-phenyl)-propionic acid methyl ester (10.6 g, 46% yield) as an oil.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 4 days
  2. extractionthe mixture was extracted with AcOEt (2×100 mL)
  3. extractionextracted with AcOEt (5×100 mL)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. filtrationfiltered
  6. customthe solvents evaporated in vacuo