HRID724833

反应详情

EQUATION

反应方程式

HRID 724833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-phenylglycine (5 g, 33 mmol) and formaldehyde (37% aqueous solution, 20 mL) in acetonitrile (100 mL) was added NaBH3CN (6.8 g) and AcOH (2 mL) and the reaction mixture was stirred at room temperature overnight. Volatiles were removed in vacuo, the residue was acidified to pH=3-4 and extracted with CHCl3 several times. The combined organic extracts were dried and concentrated to afford a crude product (5.73 g), which was purified by chromatography on silica gel (EtOAc) to afford the title compound (3.96 g, 73%).

WORKUP

后处理

  1. customVolatiles were removed in vacuo
  2. extractionextracted with CHCl3 several times
  3. customThe combined organic extracts were dried
  4. concentrationconcentrated
  5. customto afford a crude product (5.73 g), which
  6. customwas purified by chromatography on silica gel (EtOAc)