Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 1-(1-Adamantyl)methyl-2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1-Adamantylmethyl methanesulfonate | HCID 2801776 | — |
| 반응물 | N-Desmethyl Dechloro Clobazam | HCID 10824683 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(1-Adamantyl)methyl-2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine | HCID 19043402 | 18.9% |
반응 단계
Sodium hydride 80% dispersion in oil (0.07 g) was added portionwise to a solution of 2,4-dioxo-5-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine (0.5 g) in DMF (50 ml). The reaction mixture was stirred for 30 min, then a solution of 1-adamantylmethyl methanesulfonate (0.537 g) in DMF (3 ml) was added. The reaction mixture was stirred at 120° for 7 h and at 23° for 15 h, then concentrated. The residue was diluted with ethyl acetate (100 ml) washed with brine (2×30 ml) and water (50 ml), dried and concentrated "in vacuo". The crude product was purified by flash chromatography (eluting with CH-EA 1:1) to give the title compound as a white foam (0.15 g). T.l.c. CH-EA (1:1), Rf =0.42.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05486514 |
| 출처 데이터셋 | uspto-grants-1996_01 |
| ORD ID | ord-3dc95db21735450aa7930dcefac8220d |
| 출처 메모 | uspto-grants-1996_01 |