Chlorosulfonic acid → 4-(2,2-Dichloro-1,1-difluoroethoxy)-2-methyl-5-nitrobenzenesulfonyl chloride

HRID 838912ノート

反応式

HRID 838912 の反応式
[Cl:1][CH:2]([Cl:17])[C:3]([F:16])([F:15])[O:4][C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=1[N+:12]([O-:14])=[O:13].[Cl:18][S:19](O)(=[O:21])=[O:20]>>[Cl:17][CH:2]([Cl:1])[C:3]([F:15])([F:16])[O:4][C:5]1[C:6]([N+:12]([O-:14])=[O:13])=[CH:7][C:8]([S:19]([Cl:18])(=[O:21])=[O:20])=[C:9]([CH3:11])[CH:10]=1

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 203252622-(2,2-Dichloro-1,1-difluoroethoxy)-4-methyl-1-nitrobenzene

生成物 1

HCID 203252614-(2,2-Dichloro-1,1-difluoroethoxy)-2-methyl-5-nitrobenzenesulfonyl chloride

実験手順

In a 500 ml stirred reaction flask equipped with thermometer, air condenser, dropping funnel and ice water bath was placed 50 ml of chlorosulfonic acid, and, while stirring at 0° to 10° C, there was added dropwise over a one-half hour period 17.2 g of 2-(2,2-dichloro-1,1-difluoroethoxy)-4-methyl-1-nitrobenzene. After stirring for 50 hours, the reaction mixture was poured over crushed ice. The organic phase was extracted with methylene chloride, and the extract was washed with dilute bicarbonate, decolorized with charcoal and dried. Evaporation of the solvent affored 10 g of 4-(2,2-dichloro-1,1-difluoroethoxy)-2-methyl-5-nitrobenzenesulfonyl chloride as a solid melting at 60°-61° C.

後処理

  1. customreaction flask
  2. customequipped with thermometer, air condenser
  3. stirringwhile stirring at 0° to 10° C
  4. stirringAfter stirring for 50 hours
  5. additionthe reaction mixture was poured
  6. customover crushed ice
  7. extractionThe organic phase was extracted with methylene chloride
  8. washthe extract was washed with dilute bicarbonate
  9. customdried
  10. customEvaporation of the solvent affored 10 g of 4-(2,2-dichloro-1,1-difluoroethoxy)-2-methyl-5-nitrobenzenesulfonyl chloride as a solid melting at 60°-61° C.

出典と根拠

ORDレコード
ord-db0903df30ad49ebae83244e5c32ca66
出典データセット
uspto-grants-1978_06
特許番号
US04093644

反応ノート

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