Ammonia → 11-chloro-6,7-dihydro-5H,13H-quinazolino[3,2-a][1,4]benzodiazepine-5,13-dione

HRID 1448802

반응식

HRID 1448802 반응식
Cl[CH2:2][C:3]1[N:12](C2C=CC=CC=2C(OCC)=O)[C:11](=[O:24])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([Cl:25])[CH:9]=2)[N:4]=1.[NH3:26]>C(OCCO)C>[Cl:25][C:8]1[CH:7]=[CH:6][C:5]2[N:4]=[C:3]3[CH2:2][NH:26][C:11](=[O:24])[C:10]4[CH:5]=[CH:6][CH:7]=[CH:8][C:9]=4[N:12]3[C:11](=[O:24])[C:10]=2[CH:9]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 203755812-chloromethyl-3-(2-ethoxycarbonylphenyl)-6-chloro-4H-quinazolin-4-one

생성물 1

HCID 2037558511-chloro-6,7-dihydro-5H,13H-quinazolino[3,2-a][1,4]benzodiazepine-5,13-dione수율 83%

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매

실험 절차

18.9 g (0.05 mol) of 2-chloromethyl-3-(2-ethoxycarbonylphenyl)-6-chloro-4H-quinazolin-4-one and 50 ml of liquid ammonia in 150 ml of ethylene glycol monoethyl ether are heated to 60° C. for 3 hours in an autoclave. After cooling the mixture, the colourless crystals are filtered off and washed several times with methanol. 13 g (83% of theory) of 11-chloro-6,7-dihydro-5H,13H-quinazolino[3,2-a][1,4]benzodiazepine-5,13-dione are obtained.

후처리

  1. temperatureAfter cooling the mixture
  2. filtrationthe colourless crystals are filtered off
  3. washwashed several times with methanol

출처 및 근거

ORD 기록
ord-f1b179e5b6b4496785a459511e5cbbc8
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04187306

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