تفاعل #816448

معادلة التفاعل

Water

4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide

MeI

potassium carbonate

→

title compound

المردود 104.0%

4-Chloro-2-methyl-5-phenylisothiazol-3(2H)-one 1,1-dioxide

المردود 104.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىthe white precipitate formed
2. 2
   ترشيحwas filtered off
3. 3
   غسيلwashed with water
4. 4
   workup.ADDITIONToluene was added to the precipitate
5. 5
   أخرىthe mixture was evaporated
6. 6
   أخرىthe residue was dried for three days under vacuum

الإجراء التجريبي

A solution of 4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide (2.0 g, 8.21 mmol) and MeI (3.5 g, 24.6 mmol) in DMF (30 ml) was cooled with an ice bath, and anhydrous potassium carbonate (1.13 g, 8.21 mmol) was added. The mixture was then allowed to warm to rt and stirred for 21 h. Water (60 ml) was added and the white precipitate formed, was filtered off and washed with water. Toluene was added to the precipitate and the mixture was evaporated and the residue was dried for three days under vacuum to give the title compound (2.2 g, 102%) containing traces of water and toluene. 1H NMR (400 MHz, CDCl3): δ 3.23 (s, 3H), 7.52-7.56 (m, 3H), 7.86-7.88 (m, 2H); 13C-NMR (100 MHz, CD3CN): δ 24.5, 123.8, 1291, 129.5, 130.7, 133.0, 143.1, 157.6.

المصدر