4-Chloroaniline → LY 181984

HRID 326691

反応式

HRID 326691 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[C:9]1([CH3:21])[CH:14]=[CH:13][C:12]([S:15]([N:18]=[C:19]=[O:20])(=[O:17])=[O:16])=[CH:11][CH:10]=1>C(Cl)Cl>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:19]([NH:18][S:15]([C:12]2[CH:13]=[CH:14][C:9]([CH3:21])=[CH:10][CH:11]=2)(=[O:17])=[O:16])=[O:20])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 78124-ChloroanilineHCID 77703p-Toluenesulfonyl isocyanate

生成物 1

HCID 160725LY 181984収率 94.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of 6.25 g (49.00 mmoles) of 4-chloroaniline in 10 ml of methylene chloride was added to a solution of 9.85 g (49.95 mmoles) of p-toluenesulfonyl isocyanate in 75 ml of methylene chloride with stirring. The mixture became quite warm and a heavy white precipitate formed. An additional 100 ml of methylene chloride were added. The reaction mixture was stirred an additional 15 minutes, and the precipitate was recovered by filtration affording 15.0 g of the title product as a white solid. A small amount of the material was crystallized from diethyl ether to provide the title compound (87% yield) with a melting point of 174-176° C.

後処理

  1. temperatureThe mixture became quite warm
  2. customa heavy white precipitate formed
  3. stirringThe reaction mixture was stirred an additional 15 minutes
  4. filtrationthe precipitate was recovered by filtration

出典と根拠

ORDレコード
ord-c4aecccb27b64080b91bc05032c6deae
出典データセット
uspto-grants-1993_12
特許番号
US05270329

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