7-chloro-4,5-dihydro-3-(hydroxymethyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one → 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde

HRID 867559

반응식

HRID 867559 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[CH2:16][OH:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1>[O-2].[O-2].[Mn+4].C(Cl)Cl>[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[CH:16]=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 1

HCID 212899527-chloro-4,5-dihydro-3-(hydroxymethyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

생성물 1

HCID 198515847-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

18.0 g (64.8 mmol) of 7-chloro-4,5-dihydro-3-hydroxymethyl-5methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one, 75 g of manganese dioxide and 700 ml of methylene chloride are stirred at room temperature for 1.5 hours. The reaction mixture is filtered and the filtrate is evaporated. By recrystallization of the residue from alcohol there is obtained 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde of melting point 204°-205°.

후처리

  1. filtrationThe reaction mixture is filtered
  2. customthe filtrate is evaporated
  3. customBy recrystallization of the residue from alcohol

출처 및 근거

ORD 기록
ord-73709b47a02c461482d032f18ff8f961
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04775671

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