HRID595802

反应详情

EQUATION

反应方程式

HRID 595802 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 (R)-2-(3-chlorophenyl)oxirane (13 g, 84 mmol) in THF (84 mL) was added NaHMDS (1 M in THF) (252 mL, 252 mmol) slowly at 0° C. The reaction mixture was warmed up to room temperature and stirred for overnight. To the reaction mixture, water (33 mL, 2.5 mL/g) added. After stirring for 5 h at room temperature, solvent was removed in vacuo to about ¼ and partitioned by DCM. The bottom layer is a little cloudy and the top layer was a brown solution. Both layers were concentrated, which contained the desired (R)-2-amino-1-(3-chlorophenyl)ethanol (14 g, 97%). The combined products were used in next step without further purification. LCMS (m/z): 172.1 (MH+), 0.37 min.

WORKUP

后处理

  1. stirringAfter stirring for 5 h at room temperature
  2. customsolvent was removed in vacuo to about ¼
  3. custompartitioned by DCM
  4. concentrationBoth layers were concentrated
  5. customThe combined products were used in next step without further purification
  6. custom172.1 (MH+), 0.37 min.