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

HRID 16190

반응식

HRID 16190 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-ead65bc416034178bfb8f49ceb9eaf1f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737136B2

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