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Chloroform → (+/-)-trans-3-[(3-Cyclohexen-1-yl)carbonyl]-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Cyclohexene-1-carbonyl chloride | HCID 523058 | — |
| 反応物 | (+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine | HCID 86734686 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (+/-)-trans-3-[(3-Cyclohexen-1-yl)carbonyl]-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine | HCID 86734688 | — |
反応手順
Triethylamine (10 ml.) was added with stirring to a solution of 5.5 g. (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine in 100 ml. chloroform, followed by addition, with stirring, of 5.76 g. (0.04 moles) 3-cyclohexene-1-carbonyl chloride in 10 ml. chloroform. The mixture was refluxed 2 hours then cooled and water was added. The organic layer was separated, dried over K2CO3, and evaporated to dryness in vacuo. Trituration of the residual oil in hexane gave (±)-trans-3-[(3-cyclohexen-1-yl)carbonyl]-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine, m.p. 156.5°-158.5° .
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04018930 |
| 出典データセット | uspto-grants-1977_04 |
| ORD ID | ord-0a572bf32bce4963be8dbc8130dcf586 |
| 出典メモ | uspto-grants-1977_04 |