참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-(3-Chloropropyl)-2-methyl-1,3-dioxolane | HCID 80079 | — |
| 반응물 | HCID 12752824 | HCID 12752824 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 86734690 | HCID 86734690 | — |
반응 단계
3.6 grams of potassium iodide and 12 ml. of triethylamine were added to a solution of 5.5 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]=indolo[1,7-ab][1]benzazepine in 50 ml. DMF, followed by addition of 3.7 grams of 5-chloro-2-pentanone ethylene ketal. The mixture was heated at approximately 62° C for 20 hours. The mixture was then poured into water, extracted with benzene, and chromatographed through basic alumina to eliminate remaining benzazepine starting material. The resulting ketal was dissolved in ether. HCl gas was bubbled through this solution to precipitate the hydrochloride salt of the title compound. Recrystallization from ethanol yielded 350 mg. of the title compound, hydrochloride salt, m.p. 258°-259° C(dec).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04018930 |
|---|
| 출처 데이터셋 | uspto-grants-1977_04 |
|---|
| ORD ID | ord-eefc34aa945b440da2ec42f1a254114a |
|---|
| 출처 메모 | uspto-grants-1977_04 |
|---|