化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → 5,10-Dihydro-5-[3-pyrrolidino-propionyl]-11H-dibenzo[b,e][1,4]diazepin-11-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Acryloyl chloride | HCID 13140 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 5,10-Dihydro-11H-dibenzo(b,e)(1,4)diazepin-11-one | HCID 201327 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5,10-Dihydro-5-[3-pyrrolidino-propionyl]-11H-dibenzo[b,e][1,4]diazepin-11-one | HCID 12834683 | — |
反応手順
6.3 gm (0.03 mol) of 5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one and 3.3 gm (0.036 mol) of acrylic acid chloride were refluxed, while stirring, in 200 ml of toluene for 3 hours. The reaction mixture was then evaporated in vacuo. The dry residue was admixed with 200 ml of ethanol, and 2.5 gm (0.035 mol) of pyrrolidine were added dropwise, while stirring, to the boiling solution. Subsequently, the reaction mixture was heated for 20 minutes, then evaporated in vacuo to about 1/10 of its original volume, and discolored by filtration through activated charcoal/silica gel. The crude product was recrystallized from a little ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04377576 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-993854165d8f4ec4a76a748cfa519fad |
| 出典メモ | uspto-grants-1983_03 |