N,N-Dimethylaniline → 6-Chloro-2[[4-(dimethylamino)phenyl]amino]3-nitrobenzoic acid

HRID 1248839

反応式

HRID 1248839 の反応式
[CH3:1][N:2]([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.CN(C)C1C=CC=CC=1.Cl[C:21]1[C:29]([N+:30]([O-:32])=[O:31])=[CH:28][CH:27]=[C:26]([Cl:33])[C:22]=1[C:23]([OH:25])=[O:24]>ClCCl>[Cl:33][C:26]1[C:22]([C:23]([OH:25])=[O:24])=[C:21]([NH:9][C:6]2[CH:7]=[CH:8][C:3]([N:2]([CH3:10])[CH3:1])=[CH:4][CH:5]=2)[C:29]([N+:30]([O-:32])=[O:31])=[CH:28][CH:27]=1

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 7472N,N-dimethyl-p-phenylenediamineHCID 3506232,6-Dichloro-3-nitrobenzoic acid

生成物 1

HCID 135883486-Chloro-2[[4-(dimethylamino)phenyl]amino]3-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 41.0 g of N,N-dimethyl-p-phenylenediamine, 100 ml of N,N-dimethylaniline, and 23.6 g of 2,6-dichloro-3-nitrobenzoic acid was heated for seven hours on a steam bath. The resulting cake was suspended in dichloromethane, filtered, and the solid washed with water. Recrystallization from DMF-ethanol provided 6-chloro-2[[4-(dimethylamino)phenyl]amino]-3-nitrobenzoic acid, mp 222°-223° C. (dec).

後処理

  1. temperaturewas heated for seven hours on a steam bath
  2. filtrationfiltered
  3. washthe solid washed with water
  4. customRecrystallization from DMF-ethanol

出典と根拠

ORDレコード
ord-be0cc871550e43d7b1fe5ba975f8ad50
出典データセット
uspto-grants-1986_12
特許番号
US04626540

関連ノート

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