HRID926351
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 75 °C
PROCEDURE
实验过程
To a solution of 2-methyl-morpholine-3-carboxylic acid ethyl ester (Comp. No. 27) (0.180 g, 1.039 mmol) in methanol (4 ml) was added water (2 ml) and potassium hydroxide (0.291 g, 5.195 mmol). The resulting mixture was heated to 75° C. until the color turned to red. The mixture was allowed to cool to room temperature, diluted with water and acidified to pH=1 with aqueous hydrochloric acid (2 M). The solution was washed with a mixture of dichloromethane and isopropanol (3:1) and freeze-dried. The resulting white solid was used in the next step without further purification. LC/MS (method 7): Rt=0.11 min; m/z=146.20 (M+H+).
WORKUP
后处理
- temperatureto cool to room temperature
- washThe solution was washed with a mixture of dichloromethane and isopropanol (3:1)
- customfreeze-dried
- customThe resulting white solid was used in the next step without further purification