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

HRID 536052ノート

反応式

HRID 536052 の反応式
[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]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 679672,4-Difluoronitrobenzene

生成物 1

HCID 49621612,4-Difluoro-5-nitrobenzenesulfonyl chloride収率 81%

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4d29dc274b844d67b1318e46824a7a5b
出典データセット
uspto-grants-2014_10
特許番号
US08859571B2

反応ノート

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