HRID714016

反应详情

EQUATION

反应方程式

HRID 714016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
7.5 °C

PROCEDURE

实验过程

L-Homocystine (200.0 g, 745.5 mmol, 1.0 eq.) is suspended in THF (1000 mL, 5.0 vol.) and cooled to 5-10° C. Addition of 20% sodium hydroxide (521.7 mL, 626.2 g, 125.25 g at 100%, 3.13 mmol, 4.2 eq.) is followed by addition of benzyl chloroformate (220.3 mL, 267 g, 1565.5 mmol, 2.1 eq.). Conversion is complete after a night at room temperature (L-Homocystine<1%). Extractions and washings of the organic layer with water leads to a yellow oil which is isolated in quantitative yield, and which slowly crystallizes as a yellowish solid at room temperature.

WORKUP

后处理

  1. waitConversion is complete after a night at room temperature
  2. extractionExtractions and washings of the organic layer with water leads to a yellow oil which
  3. customis isolated in quantitative yield, and which
  4. customslowly crystallizes as a yellowish solid at room temperature