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Hydrogen Bromide → alpha-Hydroxyalprazolam

HRID 2296065
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HRID 2296065 반응식
COC1C=CC(C[O:8][CH2:9][C:10]2[N:14]3[C:15]4[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][C:16]=4[C:17]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)=[N:18][CH2:19][C:13]3=[N:12][N:11]=2)=CC=1.Br.[OH-].[Na+]>C(O)(=O)C>[C:20]1([C:17]2[C:16]3[CH:26]=[C:27]([Cl:30])[CH:28]=[CH:29][C:15]=3[N:14]3[C:10]([CH2:9][OH:8])=[N:11][N:12]=[C:13]3[CH2:19][N:18]=2)[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 14798Sodium HydroxideHCID 204730871-[(p-methoxybenzyloxy)-methyl]-6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine

생성물 1

HCID 162244alpha-Hydroxyalprazolam

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 3,0 g 1-[(p-methoxybenzyloxy)-methyl]-6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine in 30 ml of glacial acetic acid is added at 25° 24 ml 48% aqueous hydrobromic acid. The reaction mixture is stirred for 20 minutes, neutralised with 30% sodium hydroxide solution and extracted with methylenechloride. The organic phase is separated, washed with water, dried over sodium sulphate and evaporated to dryness. The crystallisation of the residue from acetate-ether-petrol ether yields 6-phenyl-8-chloro-4-H-s-triazolo[4,3-a][1,4]benzodiazepine-1-methanol, M.P. 209°-211°.

후처리

  1. extractionextracted with methylenechloride
  2. customThe organic phase is separated
  3. washwashed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated to dryness
  6. customThe crystallisation of the residue from acetate-ether-petrol ether

출처 및 근거

ORD 기록
ord-934559f1cee24f87a3e64acc7d5fa532
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04427590

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