化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 86734685、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Dichloro-2-butene | HCID 13556 | — |
| 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 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86734685 | HCID 86734685 | 80.4% |
反応手順
A suspension of 2.76 g of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3';2,3]indolo[1,7-ab][1]benzazepine in 20 ml of dimethylformamide (DMF) containing 2.3 ml triethylamine was treated with 1.25 g of 1,3-dichloro-2-butene. Solution resulted immediately. The solution was stirred at room temperature for 4 hours, by which time some white precipitate had formed. The reaction mixture was poured into 150 ml of cold water, a gummy solid was separated and washed by decantation with cold water. Recrystallization from ethanol gave 2.93 g of the title compound, m.p. 130°-132° C.
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-056e9fa4c4734dc388454b9a3f610f02 |
| 出典メモ | uspto-grants-1977_04 |