Water → 3-bromo-8-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

HRID 223206노트

반응식

HRID 223206 반응식
[Br:1]N1C(=O)CCC1=O.[F:9][C:10]1[CH:11]=[CH:12][C:13]2[N:19]3[CH:20]=[N:21][CH:22]=[C:18]3[CH2:17][N:16]([CH3:23])[C:15](=[O:24])[C:14]=2[CH:25]=1.O>CN(C)C=O>[Br:1][C:22]1[N:21]=[CH:20][N:19]2[C:13]3[CH:12]=[CH:11][C:10]([F:9])=[CH:25][C:14]=3[C:15](=[O:24])[N:16]([CH3:23])[CH2:17][C:18]=12

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 229145898-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

생성물 1

HCID 205232943-bromo-8-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.58 g of N-bromosuccinimide are added to 4.62 g (20 mmol) of 8-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one in 100 ml of dimethylformamide and the mixture is stirred at room temperature for 2 hours. Subsequently, the mixture is poured into 500 ml of water and extracted several times with chloroform. The combined chloroform extracts are washed with water, dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate, there is obtained 3-bromo-8-fluoro-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 200°.

후처리

  1. extractionextracted several times with chloroform
  2. washThe combined chloroform extracts are washed with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customAfter recrystallization of the residue from ethyl acetate

출처 및 근거

ORD 기록
ord-91a6051bce924c19aa6dd30ef3464c20
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04352818

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