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
- 0 °C
PROCEDURE
实验过程
1-Benzyl-3-acetylthio-azetidine (1 g, 4.518 mmol) prepared in Preparation Example 49 was dissolved in methanol (20 ml), and oxygen was completely removed by passing nitrogen through the mixture. The resulting mixture was cooled to 0° C., 2N sodium hydroxide (2.27 ml, 4.518 mmol) was added thereto slowly, stirred at 0° C. for 30 min, and then 2N—HCl was added thereto to neutralize (pH 7) the mixture. The resulting solution was concentrated under a reduced pressure, and the concentrate was dissolved in ethyl acetate, and washed with a saturated salt solution. The organic layer was dried over magnesium sulfate and concentrated under a reduced pressure to obtain 620 mg (yield: 77%) of the title compound, which was used in the next reaction without any additional purification.
WORKUP
后处理
- customoxygen was completely removed
- concentrationThe resulting solution was concentrated under a reduced pressure
- dissolutionthe concentrate was dissolved in ethyl acetate
- washwashed with a saturated salt solution
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated under a reduced pressure