HRID1870598

反应详情

EQUATION

反应方程式

HRID 1870598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of the above ketal (3.2 gm, 15 mmol) and sodium saccharin (3.1 gm, 14 mmol) in dimethylformamide (15 mL) was heated at 170° C. for 5 hours. The cooled reaction mixture was poured into water and the crude product extracted into ethyl acetate. The dried extract was evaporated and the crude product was chromotographed on a column of silica gel eluting with a gradient of 20-40% EtOAc/hexane to give crystalline 1,1-dioxido-2-(4-oxo-pentyl)-1,2-benzisothiazol-3(2H)-one, melting point 90-93° C.

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. extractionthe crude product extracted into ethyl acetate
  3. extractionThe dried extract
  4. customwas evaporated