化工社化工社 化学情報印刷レポート · 研究参考用
Cyclohexanol → Cyclohexyl Hydrogen Phenylmalonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclohexanol | HCID 7966 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Phenylmalonic acid | HCID 75791 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Cyclohexyl Hydrogen Phenylmalonate | HCID 19042990 | — |
反応手順
Phenylmalonic acid (13.5 g, 0.07 mol) in dry ether (40 mL) was treated with thionyl chloride (8.92 g, 5.4 mL, 0.07 mol) and one drop of N,N-dimethylformamide. The mixture was heated at 40°-50° C. for 3 hours. The clear solution was distilled under vacuum. The oily residue was redissolved in dry ether (40 mL), the solution was treated with cyclohexyl alcohol (0.075 mol, 7.9 mL) and refluxed for 2 hours. The mixture was worked up as before to give an oily product which crystallized on standing. Recrystallization was carried out from a benzenepetroleum ether (40°-60°) mixture to give a white crystalline product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418244 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-ac0b0d8f6fdf49b792a5870d4b32ad56 |
| 出典メモ | uspto-grants-1995_05 |