Hydrogen Bromide → alpha-Hydroxytriazolam

HRID 267225

반응식

HRID 267225 반응식
Br.COC1C=CC(C[O:9][CH2:10][C:11]2[N:15]3[C:16]4[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:17]=4[C:18]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[Cl:27])=[N:19][CH2:20][C:14]3=[N:13][N:12]=2)=CC=1.[OH-].[Na+]>C(O)(=O)C>[Cl:27][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[C:18]1[C:17]2[CH:28]=[C:29]([Cl:32])[CH:30]=[CH:31][C:16]=2[N:15]2[C:11]([CH2:10][OH:9])=[N:12][N:13]=[C:14]2[CH2:20][N:19]=1

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 14798Sodium HydroxideHCID 204730851-[(p-methoxybenzyloxy)-methyl]-6-(o-chlorophenyl)-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine

생성물 1

HCID 1963alpha-Hydroxytriazolam

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

An amount of 72 ml of 48% aqueous hydrobromic acid is added to 20° to a solution of 9.7 g of 1-[ (p-methoxybenzyloxy)-methyl]-6-(o-chlorophenyl)-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine in 90 ml of glacial acetic acid. The reaction mixture is stirred for 55 minutes; it is then neutralised with 30% sodium hydroxide solution and extracted with methylene chloride. The organic phase is separated, washed with water, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from ethyl acetate/petroleum ether yields 6-(o-chlorophenyl)-8-chloro-4 h-s-triazolo[4,3-a] [1,4]benzodiazepine-1-methanol, M.P. 235°-237°.

후처리

  1. extractionextracted with methylene chloride
  2. customThe organic phase is separated
  3. washwashed with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation
  6. customCrystallisation of the residue from ethyl acetate/petroleum ether

출처 및 근거

ORD 기록
ord-c916bc4dd7264334ac786fec36a6f8ea
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941799

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