2-Bromoethyldimethylamine → 4-(2-Dimethylaminoethyl)-1-methyl-8-chloro-6-phenyl-4H-s-triazolo[4,3-a] [1,5]benzodiazepin-5-one

HRID 261178ノート

反応式

HRID 261178 の反応式
[CH3:1][C:2]1[N:6]2[C:7]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:8]=3[N:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:10](=[O:12])[CH2:11][C:5]2=[N:4][N:3]=1.[H-].[Na+].[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29]Br>COCCOC>[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][CH:11]1[C:10](=[O:12])[N:9]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:8]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:7]=2[N:6]2[C:2]([CH3:1])=[N:3][N:4]=[C:5]12

参加物

5

反応物 3

HCID 178642-BromoethyldimethylamineHCID 24758Sodium hydrideHCID 122643201-methyl-8-chloro-6-phenyl-4H-s-triazolo-[4,3-a][1,5]benzodiazepin-5-one

生成物 1

HCID 203293314-(2-Dimethylaminoethyl)-1-methyl-8-chloro-6-phenyl-4H-s-triazolo[4,3-a] [1,5]benzodiazepin-5-one

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

37.0 g of 1-methyl-8-chloro-6-phenyl-4H-s-triazolo[4,3-a][1,5]benzodiazepin-5-one and 7.8 g of a 50 percent sodium hydride mineral oil dispersion in 400 ml of dry 1,2-dimethoxyethane are stirred for 2 hours. A solution of 13.7 g of 2-dimethylaminoethyl bromide in 40 ml of dry 1,2-dimethoxyethane is added and the whole is stirred for 18 hours. The solvent is evaporated and the residue is partitioned between methylene chloride and water. The organic phase is washed with water, dried and evaporated to give the title compound.

後処理

  1. customThe solvent is evaporated
  2. customthe residue is partitioned between methylene chloride and water
  3. washThe organic phase is washed with water
  4. customdried
  5. customevaporated

出典と根拠

ORDレコード
ord-9494fb4d7cc7460cbcf04c64e5b4ea2b
出典データセット
uspto-grants-1979_08
特許番号
US04164498

反応ノート

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