HRID2120009

反应详情

EQUATION

反应方程式

HRID 2120009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A recovery flask was charged with 520 mg (2.81 mmol) of the optically active 1-(4-fluorophenyl)-2-nitroethanol obtained in Example 14, 52 mg of 10% Pd/C, and 2.8 ml of methanol, and stirring was carried out under an atmosphere of hydrogen at atmospheric pressure and 30° C. for 22 hours. After the reaction was completed, the catalyst was filtered off and the solvent was distilled off under vacuum to give 421 mg (yield 97%, 1H-NMR) of optically active 2-amino-1-(4-fluorophenyl)ethanol as white crystals. The amino group of the amino alcohol so obtained was monobenzoylated by reaction with benzoyl chloride, and when it was analyzed using a CHIRALCEL OD column (eluant; n-hexane:2-propanol=30:1), it was found that the optical purity was 96% ee.

WORKUP

后处理

  1. filtrationthe catalyst was filtered off
  2. distillationthe solvent was distilled off under vacuum