Dimethylformamide → 2-[(3,4-dichlorophenyl)amino]ethanesulfonyl Fluoride

HRID 2351866ノート

反応式

HRID 2351866 の反応式
CN(C)C=O.[Cl:6][C:7]1[CH:8]=[C:9]([CH:11]=[CH:12][C:13]=1[Cl:14])[NH2:10].[CH:15]([S:17]([F:20])(=[O:19])=[O:18])=[CH2:16]>O>[Cl:6][C:7]1[CH:8]=[C:9]([NH:10][CH2:16][CH2:15][S:17]([F:20])(=[O:19])=[O:18])[CH:11]=[CH:12][C:13]=1[Cl:14]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 72573,4-DichloroanilineHCID 69612Ethenesulfonyl fluoride

生成物 1

HCID 47381922-[(3,4-dichlorophenyl)amino]ethanesulfonyl Fluoride

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A N,N-dimethylformamide solution (DMF, 100 ml) of 3,4-dichloroaniline (6.48 g, 40 mmol) and ethenesulfonyl fluoride (6.7 g, 57.9 mmol) was warmed to 110° C. for three hours. The cooled dark solution was diluted to 400 ml with water and the resulting dark oily precipate was decanted from the supernatant layer. This layer was extracted with ether (4×50 ml). The combined ether extracts were added to the oily precipitate and this dark solution was washed with brine and dried over MgSO4. The organic solution was evaporated to give the crude 2-[(3,4-dichlorophenyl)amino]ethanesulfonyl fluoride as a dark liquid in quantitative yield.

後処理

  1. customthe resulting dark oily precipate was decanted from the supernatant layer
  2. extractionThis layer was extracted with ether (4×50 ml)
  3. additionThe combined ether extracts were added to the oily precipitate
  4. washthis dark solution was washed with brine
  5. dry with materialdried over MgSO4
  6. customThe organic solution was evaporated

出典と根拠

ORDレコード
ord-bd90fc6bb6bd479d855c74b35a1f492e
出典データセット
uspto-grants-1989_10
特許番号
US04874771

反応ノート

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