HRID843283

反应详情

EQUATION

反应方程式

HRID 843283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

A solution of N-tert-butoxycarbonyl-3(S)-amino-2(R)-hydroxy-4-phenylbutyric acid methyl ester 154.7 g dissolved in ethanol 300 ml was kept at 5-15° C. and mixed with sodium borohydride 24.6 g and stirred at 15-45° C. for 3hrs. The reaction solution was cooled and adjusted with 3N-HCl to pH 2.5-3.5. Water was added to the resultant solution and then the obtained solution was cooled to 5° C. or lower to deposit crystals. The crystals were filtered, dissolved in ethyl acetate, and washed with aqueous 5% sodium bicarbonate solution to separate an organic phase, which was washed with aqueous 10% sodium chloride solution and concentrated under an reduced pressure to obtain the crude N-tert-butoxycarbonyl-3(S)-amino-2(R)-hydroxy-4-phenyl-1-butanol.

WORKUP

后处理

  1. customwas kept at 5-15° C.
  2. temperatureThe reaction solution was cooled
  3. temperaturethe obtained solution was cooled to 5° C.
  4. filtrationThe crystals were filtered
  5. dissolutiondissolved in ethyl acetate
  6. washwashed with aqueous 5% sodium bicarbonate solution
  7. customto separate an organic phase, which
  8. washwas washed with aqueous 10% sodium chloride solution
  9. concentrationconcentrated under an reduced pressure