Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Bromide → alpha-Hydroxytriazolam
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Bromide | HCID 260 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-[(p-methoxybenzyloxy)-methyl]-6-(o-chlorophenyl)-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine | HCID 20473085 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | alpha-Hydroxytriazolam | HCID 1963 | — |
반응 단계
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°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US03941799 |
| 출처 데이터셋 | uspto-grants-1976_03 |
| ORD ID | ord-c916bc4dd7264334ac786fec36a6f8ea |
| 출처 메모 | uspto-grants-1976_03 |