Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → 10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-(10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepin-10-yl)-2,2,2-trifluoroethanone | HCID 22135236 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepine | HCID 22135237 | 94.7% |
반응 단계
1-(10,11-Dihydro-5-methyl-dibenzo[b,e][1,4]diazepin-10-yl)-2,2,2-trifluoroethanone of Step B (1.0 g) in ethanol (25 mL) was treated with 1 N sodium hydroxide (10 mL). The reaction mixture was refluxed for five hours, cooled, all volatiles removed in vacuo and the residue triturated with water. The resulting solid was filtered off, redissolved in dichloromethane and dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® which was eluted with several additional volumes of dichloromethane. The total effluent was evaporated to dryness to provide the title compound as an off-white crystalline solid (0.65 g), m.p. 115-117° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07329653B2 |
| 출처 데이터셋 | uspto-grants-2008_02 |
| ORD ID | ord-4d70bcf959aa474cad6d36367756485a |
| 출처 메모 | uspto-grants-2008_02 |