HRID1158242
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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. Disopropyl 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
- stirringunder stirring at −4° C
- stirringThe solution was stirred at room temperature for 18 hours
- custommethanol was removed under reduced pressure
- additionDisopropyl ether (90 mL) was added to the precipitated crystals, which
- filtrationwere filtered
- washwashed twice with diisopropyl ether (30 mL)