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p-Toluenesulfonic acid → 4-Propyl-cyclohexanecarboxylic acid 4-acryloyloxy-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4-Hydroxybutyl acrylate | HCID 75588 | — |
| 反応物 | (1s,4r)-4-Propylcyclohexane-1-carboxylic acid | HCID 1490324 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Propyl-cyclohexanecarboxylic acid 4-acryloyloxy-butyl ester | HCID 59289090 | — |
反応手順
4-Propyl-cyclohexanecarboxylic acid (10.0 g, 58.0 mmol), 4-hydroxybutyl acrylate (8.0 g, 57.0 mmol) and a catalytic amount of para-toluene sulphonic acid are stirred under reflux in toluene (100 ml) in a flask equipped with Dean-Stark apparatus. The reaction is shown to be complete by GCMS after 1 hour. The solution is allowed to cool to room temperature, is washed with aqueous sodium carbonate and water, dried and evaporated to dryness. Purification is achieved by flash column chromatography using petrol as eluant. Evaporation of the appropriate fractions gives a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08372307B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-a2e30c497dba4744a6945527d75788a1 |
| 出典メモ | uspto-grants-2013_02 |