反应 #1810820

反应方程式

HCl

sodium sulfite

2-chloro-5-fluorosulfonyl-benzoic acid

NaOH

→

title compound

收率 76.5%

2-Chloro-5-sulfino-benzoic acid

收率 76.5%

溶剂

water

water

反应条件

后处理

1. 1
   其他was removed under vacuum
2. 2
   workup.ADDITIONMethanol was added
3. 3
   过滤the precipitate filtered off
4. 4
   浓缩the filtrate concentrated
5. 5
   workup.ADDITIONMethanol and diethylether were added
6. 6
   过滤the precipitate was filtered off
7. 7
   洗涤washed with ether
8. 8
   其他dried

实验过程

A solution of 33.59 g (267 mmol) sodium sulfite in 100 ml water at 0° C. is treated with 21.2 g (89 mmol) 2-chloro-5-fluorosulfonyl-benzoic acid and 26.6 ml of a 10 M aqueous NaOH solution (267 mmol). The mixture was allowed to stir for 3 h at room temperature, acidified with HCl conc. (pH=4) and water was removed under vacuum. Methanol was added, the precipitate filtered off and the filtrate concentrated. Methanol and diethylether were added and the precipitate was filtered off washed with ether and dried to yield 15 g (76.5%) of the title compound as white gum. MS (m/e): 219.1 (M−H, 100%)

来源