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

HRID 261236노트

반응식

HRID 261236 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-48808cb63b8347cbbc8304689ba19aa0
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04164580

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