N-(2-Amino-4-chlorophenyl)anthranilic acid → 8-chloro-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

HRID 16190

反応式

HRID 16190 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12](O)=[O:13]>C1(C)C(C)=CC=CC=1>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]2[NH:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:13])[NH:1][C:2]=2[CH:7]=1

参加物

3

反応物 1

HCID 610730N-(2-Amino-4-chlorophenyl)anthranilic acid

生成物 1

HCID 36531168-chloro-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A solution of 2-[(2-amino-4-chlorophenyl)amino]benzoic acid (11.8 g, 45 mmol) in xylene (150 mL) was heated to reflux in a Dean-Stark apparatus. The reaction mixture was stirred at reflux temperature for 31 h. After removal of the xylene in vacuo, the title compound was obtained. There was still starting material present. Therefore the product was dissolved in xylene (150 mL) again and stirring was continued overnight at reflux temperature in a Dean-Stark apparatus. After removal of the xylene under reduced pressure the title compound (12.4 g, 50.6 mmol) was obtained.

後処理

  1. temperatureto reflux in a Dean-Stark apparatus
  2. temperatureat reflux temperature for 31 h
  3. customAfter removal of the xylene in vacuo

出典と根拠

ORDレコード
ord-ead65bc416034178bfb8f49ceb9eaf1f
出典データセット
uspto-grants-2010_06
特許番号
US07737136B2

関連ノート

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