HRID1925481

反应详情

EQUATION

反应方程式

HRID 1925481 的结构方程式

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

Thionyl chloride (47.7 mL) was added dropwise to methanol (300 mL) under stirring at −5° C. over 2 hours and 15 minutes. D-Norvaline (35.00 g) was added to the resulting light yellow solution under stirring at −4° C. The solution was stirred at room temperature for 18 hours and then methanol was removed under reduced pressure. Diisopropyl ether (90 mL) was added to the precipitated crystals, which were filtered and washed twice with diisopropyl ether (30 mL) to give (R)-norvaline methyl ester (47.74 g, 95% yield) as a white powder.

WORKUP

后处理

  1. stirringunder stirring at −4° C
  2. stirringThe solution was stirred at room temperature for 18 hours
  3. custommethanol was removed under reduced pressure
  4. additionDiisopropyl ether (90 mL) was added to the precipitated crystals, which
  5. filtrationwere filtered
  6. washwashed twice with diisopropyl ether (30 mL)