HRID1879471

反应详情

EQUATION

反应方程式

HRID 1879471 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

To a stirred solution of 2-(3-cyano-benzyl)-1,1-dioxo-1λ6-isothiazolidine-3-carboxylic acid methyl ester (6.0 g, 20.4 mmol) in a tetrahydrofuran-water mixture (4:1, 50 mL), lithium hydroxide monohydrate (2.5 g, 59.6 mmol) was added at room temperature and stirred at this temperature for 4 h. Then tetrahydrofuran was removed from the reaction mixture under reduced pressure. The residual reaction mixture was cooled to 0° C. and 1N hydrochloric acid was added to make the pH˜2. The acidified reaction mixture was extracted with ethyl acetate (3×150 mL). The combined organic layers were washed with water (2×50 mL) followed by brine (50 mL) and then dried over sodium sulfate and concentrated under reduced pressure to provide 2-(3-cyano-benzyl)-1,1-dioxo-1λ6-isothiazolidine-3-carboxylic acid (5.2 g, 91%).

WORKUP

后处理

  1. customThen tetrahydrofuran was removed from the reaction mixture under reduced pressure
  2. customThe residual reaction mixture
  3. customThe acidified reaction mixture
  4. extractionwas extracted with ethyl acetate (3×150 mL)
  5. washThe combined organic layers were washed with water (2×50 mL)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure