تفاعل #816447

معادلة التفاعل

DMF

oxalyl chloride

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

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title compound

المردود 50.0%

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

المردود 50.0%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe resulting solution was heated
2. 2
   درجة الحرارةunder reflux until it
3. 3
   ترشيحfiltered

الإجراء التجريبي

Dry DMF (1.2 ml) was added dropwise to a mixture of oxalyl chloride (4.96 g, 39.1 mmol) and 4-hydroxy-5-phenylisothiazol-3(2H)-one 1,1-dioxide (2.2 g, 9.77 mmol) in DCM. The resulting solution was heated under reflux until it turned orange. The mixture was then cooled to room temperature and filtered affording the title compound (1.18 g, 50%) as white solid. 1H NMR (400 MHz, d6-DMSO): δ 7.41-7.54 (m, 3H), 7.77-7.80 (m, 2H), 12.70 (br.s, 1H); 13C-NMR (100 MHz, d6-DMSO): δ 126.1, 127.1, 128.3, 129.9, 130.6, 144.9, 162.2.

المصدر