HRID1443764

反应详情

EQUATION

反应方程式

HRID 1443764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customoxygen was completely removed
  2. concentrationThe resulting solution was concentrated under a reduced pressure
  3. dissolutionthe concentrate was dissolved in ethyl acetate
  4. washwashed with a saturated salt solution
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under a reduced pressure