HRID1587982

反应详情

EQUATION

反应方程式

HRID 1587982 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add 4-benzyloxycarbonylamino-2(S)-hydroxybutyric acid (2.57 g) to absolute ethanol (30 ml) containing thionyl chloride (2.0 ml) and heat the resulting mixture under reflux for 20 hours. Cool, filter and concentrate the reaction mixture in vacuo to give a pale yellow oil. Chromatograph this oil on a column of silica gel (500 ml) using ethyl acetate as eluant to obtain a yellow oil, [α]D26 =+0.4° (MeOH). Hydrogenate the product (1.4 g) in absolute ethanol (50 ml) containing 10% Pd/C (0.50 g) at 50 psi for 2 hours. Filter the mixture and concentrate the mixture in vacuo to give the title compound as an oil.

WORKUP

后处理

  1. temperatureheat the resulting mixture
  2. temperatureunder reflux for 20 hours
  3. temperatureCool
  4. filtrationfilter
  5. concentrationconcentrate the reaction mixture in vacuo
  6. customto give a pale yellow oil
  7. filtrationFilter the mixture
  8. concentrationconcentrate the mixture in vacuo