化工社化工社 化学情報印刷レポート · 研究参考用
Cyclohexene → 3-Methyl-2,3,4,5,6,7-hexahydro-1H-inden-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclohexene | HCID 8079 | — |
| 反応物 | Crotonic Acid | HCID 637090 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Methyl-2,3,4,5,6,7-hexahydro-1H-inden-1-one | HCID 11105531 | 66% |
反応手順
Cyclohexene (27.3 g, 0.33 mol), crotonic acid (28.7 g, 0.33 mol) and polyphosphoric acid (300 mL) were mechanically stirred under a nitrogen atmosphere at 60° C. for 30 minutes. The slurry was poured into water and the aqueous solution extracted with diethyl ether. The diethyl ether extract was washed successively with a 10 percent NaHCO3 solution and a saturated NaCl solution. The organic extract was dried over anhydrous MgSO4. The solution was filtered and the solvent removed under reduced pressure. The crude product was purified via vacuum distillation (bp 87°-92° C. at 5 mm) to give 32.6 g (66 percent) of purified material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624878 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-13f364340a054d92b2099797681aaa0c |
| 出典メモ | uspto-grants-1997_04 |