Chlorosulfonic acid → 3-(2-Chloroacetamido)-2,4-dimethylbenzene-1-sulfonyl chloride
반응식
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH3:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:8]=1[NH:14][C:15]([CH2:17][Cl:18])=[O:16]>>[Cl:18][CH2:17][C:15]([NH:14][C:8]1[C:7]([CH3:6])=[C:12]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:11]=[CH:10][C:9]=1[CH3:13])=[O:16]참가 물질
3
실험 절차
To chlorosulfonic acid (75 mL, 1.15 mol) was added with stirring solid 2-chloro-2',6'-acetoxylidide over a 30 minute period at 25°-30° C. and the reaction mixture was stirred at 60°-65° C. for 1.5 hours. The reaction was cooled, added to ice and extracted with ethyl acetate/methyl ethyl ketone. The combined extracts were washed with water and brine; dried, and the solvent was removed in vacuo; the residual product (61.4 g, 69%) was a white solid, m.p. 147.5°-149° C.
후처리
- temperatureThe reaction was cooled
- additionadded to ice
- extractionextracted with ethyl acetate/methyl ethyl ketone
- washThe combined extracts were washed with water and brine
- customdried
- customthe solvent was removed in vacuo
출처 및 근거
- ORD 기록
- ord-fcb52f6862044265a9b0a66524a07ab6
- 출처 데이터셋
- uspto-grants-1991_01
- 특허 번호
- US04988604
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