Chlorosulfonic acid → 2,4-Difluoro-5-nitrobenzenesulfonyl chloride

HRID 536052노트

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HRID 536052 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[Cl:12][S:13](O)(=[O:15])=[O:14]>>[F:8][C:6]1[CH:7]=[C:2]([F:1])[C:3]([N+:9]([O-:11])=[O:10])=[CH:4][C:5]=1[S:13]([Cl:12])(=[O:15])=[O:14]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 679672,4-Difluoronitrobenzene

생성물 1

HCID 49621612,4-Difluoro-5-nitrobenzenesulfonyl chloride수율 81%

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온도
100 °C

실험 절차

A mixture of 2,4-difluoro-1-nitrobenzene (20 g, 126 mmol) in chlorosulfonic acid (44 g, 378 mmol) was stirred at 100° C. for 48 hours before being poured into ice-water and extracted with EtOAc. The organic extract was dried (Na2SO4) and concentrated, and the residue was triturated with 10% EtOAc-petroleum ether to give 2,4-difluoro-5-nitrobenzenesulfonyl chloride as a brown oil (21 g, 81%) which was used directly in the next step.

후처리

  1. extractionextracted with EtOAc
  2. extractionThe organic extract
  3. dry with materialwas dried (Na2SO4)
  4. concentrationconcentrated
  5. customthe residue was triturated with 10% EtOAc-petroleum ether

출처 및 근거

ORD 기록
ord-4d29dc274b844d67b1318e46824a7a5b
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859571B2

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