تفاعل #816435

معادلة التفاعل

Oxalyl chloride

2-ethyl-4-hydroxy-5-[4-(trifluoromethyl)phenyl]isothiazol-3(2H)-one 1,1-dioxide

DMF

→

title compound

المردود 71.0%

4-Chloro-2-ethyl-5-[4-(trifluoromethyl)phenyl]isothiazol-3(2H)-one 1,1-dioxide

المردود 71.0%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was refluxed for 1 h
2. 2
   أخرىIt was evaporated
3. 3
   workup.ADDITIONwater was added
4. 4
   استخلاصThe resulting mixture was extracted with EtOAc
5. 5
   غسيلthe combined organic layers were washed with brine
6. 6
   أخرىevaporated

الإجراء التجريبي

Oxalyl chloride (0.379 g, 2.99 mmol) was added dropwise to a solution of 2-ethyl-4-hydroxy-5-[4-(trifluoromethyl)phenyl]isothiazol-3(2H)-one 1,1-dioxide (0.480 g, 1.49 mmol) and DMF (0.109 g, 1.49 mmol) in DCM (12 mL). The mixture was refluxed for 1 h. It was evaporated and water was added. The resulting mixture was extracted with EtOAc, and the combined organic layers were washed with brine and evaporated to give the title compound (0.306 g, 71%) as a solid; 1H NMR (500 MHz, DMSO-d6): δ 8.07-8.11 (m, 4H), 3.81 (q, 2H), 1.33 (t, 3H).

المصدر