반응 #57431

반응 방정식

o-nitroaniline-p-sulfonic acid sodium salt

phosphoryl chloride

→

o-nitroaniline-p-sulfonyl chloride

수율 87.1%

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   workup.ADDITIONthe reaction mixture was carefully added to a large excess of ice
3. 3
   workup.STIRRINGThe resulting slurry was stirred for 15 min.
4. 4
   여과filtered
5. 5
   기타dried under vacuum

실험 절차

A mixure of o-nitroaniline-p-sulfonic acid sodium salt (25.00 g, 104 mmol) and phosphoryl chloride (75 mL, 804 mmol) under Argon was heated to reflux and vigorously stirred for 4 hours. After cooling to ambient temperature, the reaction mixture was carefully added to a large excess of ice. The resulting slurry was stirred for 15 min., filtered and dried under vacuum to provide o-nitroaniline-p-sulfonyl chloride (21.43 g, 87%) as a yellow solid. H1-NMR (dimethylsulfoxide-D6): 5.8 (b, 2H), 6.97 (d, 1H, J=8.8), 7.57 (m, 1H), 8.18 (d, 1H, J=2.0).

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