化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropylethylamine → 1-(3-Methanesulfonyl-benzoyl)-piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Methanesulfonylbenzoic acid | HCID 220380 | — |
| 反応物 | PyBroP | HCID 2733179 | — |
| 反応物 | 4-Piperidone hydrochloride | HCID 3084851 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(3-Methanesulfonyl-benzoyl)-piperidin-4-one | HCID 22397490 | 93% |
反応手順
PyBrOP™ (17.3 g) was added to a stirred mixture of 3-methanesulphonyl benzoic acid (7.35 g), 4-piperidone hydrochloride (5 g) and Hunig's base (25 ml) in dichloromethane (250 ml) with stirring at RT. The mixture was stirred overnight then washed with saturated NaHCO3 solution (200 ml) and then with saturated brine (200 ml). The organic layer was evaporated and the resulting residue purified by column chromatography (silica, 1:1 ethyl acetate: dichloromethane) to give the product as a thick oil (9.6 g; MS: APCI+(M+H) 282).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06903115B2 |
| 出典データセット | uspto-grants-2005_06 |
| ORD ID | ord-794991a1481949d1bd2934287f166b06 |
| 出典メモ | uspto-grants-2005_06 |