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Sulfuric Acid → Methyl 4-methoxycyclohexane-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Rac-(1r,4r)-4-methoxycyclohexane-1-carboxylic acid | HCID 736153 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 4-methoxycyclohexane-1-carboxylate | HCID 53849879 | — |
反応手順
1.8 ml of concentrated sulphuric acid were added to a solution of 4.00 g (25.3 mmol) of 4-methoxycyclohexanecarboxylic acid in 32 ml of methanol, and the resulting reaction solution was heated under reflux overnight. The mixture was cooled to room temperature and the pH was adjusted to 7-8 using saturated aqueous sodium bicarbonate solution. The mixture was then extracted three times with 70 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate and filtered, and the solvent was removed under reduced pressure. The crude product corresponded to the title compound. Yield: 4.30 g (99% of theory)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434690B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-10af66dab0b346579972b559ef70da67 |
| 出典メモ | uspto-grants-2016_09 |