化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → (4-Dimethylamino-4-phenylcyclohexylidene)acetic acid hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | (4-Dimethylamino-4-phenylcyclohexylidene)acetic acid methyl ester hydrochloride | HCID 67386135 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (4-Dimethylamino-4-phenylcyclohexylidene)acetic acid hydrochloride | HCID 67386703 | 98% |
反応手順
1.7 M KOH (70.5 ml, 120 mmol) was added to a solution of (4-dimethylamino-4-phenylcyclohexylidene)acetic acid methyl ester hydrochloride (1.8 g, 5.8 mmol) in ethanol (200 ml) and the mixture was stirred at RT for 16 h. The reaction mixture was concentrated and the residue was taken up in water (40 ml). The aqueous phase was extracted by shaking with ether (2×40 ml), and 5.5 M hydrochloric acid (23.6 ml, 130 mmol) was added. After the aqueous phase had been concentrated, the residue was extracted with ethanol (2×40 ml), the potassium chloride which remained was separated off and the filtrate was concentrated. The hydrochloride of the acid was thereby obtained as a colourless solid in a yield of 98% (1.67 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08017630B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-c1b813893309407887b16d63fe4d1012 |
| 出典メモ | uspto-grants-2011_09 |