تفاعل #1810820

معادلة التفاعل

HCl

sodium sulfite

2-chloro-5-fluorosulfonyl-benzoic acid

NaOH

→

title compound

المردود 76.5%

2-Chloro-5-sulfino-benzoic acid

المردود 76.5%

المذيبات

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىwas removed under vacuum
2. 2
   workup.ADDITIONMethanol was added
3. 3
   ترشيحthe precipitate filtered off
4. 4
   تركيزthe filtrate concentrated
5. 5
   workup.ADDITIONMethanol and diethylether were added
6. 6
   ترشيحthe precipitate was filtered off
7. 7
   غسيلwashed with ether
8. 8
   أخرىdried

الإجراء التجريبي

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%)

المصدر