Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 5,6-Dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | (Dimethyl sulfide)trihydroboron | HCID 12423031 | — |
| 반응물 | 5,6-dihydro-4H-[1,2,4]-triazolo-[4,3-a][1,5]benzodiazepin-5-one | HCID 21837128 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5,6-Dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine | HCID 21837004 | — |
반응 단계
A mixture of 7.0 g of 5,6-dihydro-4H-[1,2,4]-triazolo-[4,3-a][1,5]benzodiazepin-5-one in 25 ml of tetrahydrofuran is added 9 ml of 10M borane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 6 hours, cooled to room temperature and 25 ml of methanol added dropwise. The volatiles are removed under vacuum and to the residue is added 100 ml of 2N sodium hydroxide. The mixture is refluxed for 5 hours, chilled and extracted with dichloromethane. The extract is washed with 2N citric acid, water and dried (Na2SO4). The solvent is removed under vacuum to give a solid. The solid is purified by chromatography on silica gel to give the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05733905 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-44ee38b3384d451c8b68f82532c2510d |
| 출처 메모 | uspto-grants-1998_03 |