関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 6-Methoxy-alpha-tetralone | HCID 14112 | — |
| 反応物 | 2,6-Dimethylmorpholine hydrochloride | HCID 19374754 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Methoxy-2-(2,6-dimethylmorpholinomethyl)-1,2,3,4-tetrahydronaphthalen-1-one | HCID 13770569 | — |
反応手順
6-Methoxy-1,2,3,4-tetrahydronaphthalen-1-one (17.6 g, 0.1 mol), 2,6-dimethylmorpholine hydrochloride (15.1 g, 0.1 mol), and paraformaldehyde (6.0 g, 0.2 mol) were refluxed together in ethanol (50 ml) with concentrated hydrochloric acid (0.25 ml) as a catalyst for 3 hours. The reaction was cooled and poured into water containing concentrated hydrochloric acid (5 ml) and extracted with ether (200 ml). The aqueous solution was cooled in ice and neutralised with sodium hydroxide solution (10%) then extracted with ether (2×200 ml) dried over magnesium sulphate and evaporated under reduced pressure to give a residue which was recrystallised from petrol (60°-80°) to give 6-methoxy-2-(2,6-dimethylmorpholinomethyl)-1,2,3,4-tetrahydronaphthalen-1-one a white crystalline solid (10 g, 33% yield) melting at 110° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04785006 |
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| 出典データセット | uspto-grants-1988_11 |
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| ORD ID | ord-b4e037832f3844949cd1d2460ced76f7 |
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| 出典メモ | uspto-grants-1988_11 |
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