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p-Toluenesulfonic acid → HCID 59289068、化合物
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-Bromobutanol | HCID 118388 | — |
| 反応物 | (1s,4r)-4-Propylcyclohexane-1-carboxylic acid | HCID 1490324 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 59289068 | HCID 59289068 | — |
反応手順
4-Propyl-cyclohexanecarboxylic acid (10.0 g, 58.0 mmol), 4-bromobutan-1-ol (9.2 g, 60.0 mmol) and a catalytic amount of para-toluene sulphonic acid are stirred under reflux in toluene (300 ml) in a flask equipped with Dean-Stark apparatus over night. 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 4-propyl-cyclohexanecarboxylic acid 4-bromo-butyl ester as the product. The structure is confirmed by 1H NMR spectroscopy and GCMS.
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-e569159be1f043a180086ddbee91d01a |
| 出典メモ | uspto-grants-2013_02 |