Water → 3,7-dichloro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

HRID 223199노트

반응식

HRID 223199 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:17])[N:9]([CH3:16])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][CH:15]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[Cl:18]N1C(=O)CCC1=O.O>CN(C)C=O>[Cl:18][C:15]1[N:14]=[CH:13][N:12]2[C:6]3[CH:5]=[CH:4][CH:3]=[C:2]([Cl:1])[C:7]=3[C:8](=[O:17])[N:9]([CH3:16])[CH2:10][C:11]=12

참가 물질

5

반응물 3

HCID 962WaterHCID 31398ChlorosuccinimideHCID 19851597HCID 19851597, 화합물

생성물 1

HCID 205232863,7-dichloro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.30 g (5.25 mmol) of 7-chloro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one are stirred at 90° for 30 minutes in 10 ml of dimethylformamide with 800 mg (6 mmol) of N-chlorosuccinimide. Subsequently, the mixture is poured into water and extracted with chloroform. The combined chloroform extracts are washed with water, dried over magnesium sulphate and evaporated. By column chromatography on silica gel there is obtained 3,7-dichloro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 211°-212°.

후처리

  1. extractionextracted with chloroform
  2. washThe combined chloroform extracts are washed with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated

출처 및 근거

ORD 기록
ord-3da3d651636844fe8ba6836aa51b3d8a
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04352818

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