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Hydrochloric Acid → 4-(3,4-dihydro-6,7-dimethoxy-1-methyl-1H-2-benzopyran-1-yl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,4-Dimethoxyphenethyl alcohol | HCID 81911 | — |
| 反応物 | 1-(Piperidin-4-yl)ethan-1-one | HCID 2723764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(3,4-dihydro-6,7-dimethoxy-1-methyl-1H-2-benzopyran-1-yl)piperidine | HCID 20087946 | 86.5% |
反応手順
A mixture of 200 g of 3,4-dimethoxybenzeneethanol and 163.7 g of 1-(4-piperidinyl)ethanone in 800 ml of ethanol saturated with anhydrous hydrochloric acid was stirred for 15 h at ambient temperature. The mixture was concentrated under vacuum, and the concentrate was diluted with 500 ml of ethanol after which the hydrochloride precipitated. After filtration the hydrochloride was dissolved in water and sodium hydroxide until the pH was 12. The base was extracted with dichloromethane, and the organic phase was washed with water, dried and evaporated to yield 251 g (86.5%) of crude 4-(3,4-dihydro-6,7-dimethoxy-1-methyl-1H-2-benzopyran-1-yl)piperidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05393759 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-23dfc06720c841b1a7f789db27249f50 |
| 出典メモ | uspto-grants-1995_02 |