Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,2-Dibromopropane | HCID 11658 | — |
| 반응물 | 6,11-Dihydro-N-methyl-5H-dibenz(b,e)azepine-6-methanamine | HCID 13037912 | — |
| 생성물 | 2,3,4,5,11,15b-Hexahydro-2-methyl-1H-dibenz[3,4:6,7]azepino[1,2-a][1,4]diazepine | HCID 13201019 | — |
반응 단계
4.76 g 5,6-dihydro-6-methylaminomethyl-11H-dibenzo[b,e]azepine is dissolved in 125 ml dibromopropane and 5 ml triethylamine is added to the solution. The mixture is boiled under reflux with stirring for 2 hours, after which it is cooled. 150 ml Water is then added and the whole is shaken for a little while, after which the aqueous layer is separated from the dibromopropane layer. The organic layer is subsequently dried over sodium sulphate and evaporated to dryness under vacuum. The residue is further purified chromatographically on a silica gel column with methanol:acetone (9:1) as eluent.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04224321 |
| 출처 데이터셋 | uspto-grants-1980_09 |
| ORD ID | ord-b9c6f2a81adb4f1a8cfe5312e711565d |
| 출처 메모 | uspto-grants-1980_09 |