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

HRID 223206ノート

反応式

HRID 223206 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-91a6051bce924c19aa6dd30ef3464c20
出典データセット
uspto-grants-1982_10
特許番号
US04352818

反応ノート

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