Hydrogen Bromide → alpha-Hydroxytriazolam

HRID 267225

反応式

HRID 267225 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 1963alpha-Hydroxytriazolam

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-c916bc4dd7264334ac786fec36a6f8ea
出典データセット
uspto-grants-1976_03
特許番号
US03941799

関連ノート

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