化工社化工社 化学情報印刷レポート · 研究参考用
4-Chlorobutyryl chloride → 5-(4-Chlorobutyryl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | 5,10-Dihydro-11H-dibenzo(b,e)(1,4)diazepin-11-one | HCID 201327 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-(4-Chlorobutyryl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one | HCID 53856317 | — |
反応手順
A mixture of 4-chlorobutyryl chloride (3.5 g) and 10,11-dihydrodibenzo[b,e][1,4]diazepin-11-one (4.2 g) (J. Med. Chem., 1963, 6, 767) in acetone (90 ml) was heated under reflux for 8 hours and evaporated. The residue was purified by chromatography on silica using hexane plus 0-100% dichloromethane as eluant. Appropriate fractions were combined and evaporated and the residue triturated with hexane/dichloromethane to give the title compound as a colourless solid, 1.62 g (26%), m.p. 151°-152° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418229 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-79eaf72784de43c4af5c7a91e5d67ae8 |
| 出典メモ | uspto-grants-1995_05 |