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4-Hydroxy-2,2,6,6-tetramethylpiperidine → 2,2,6,6-Tetramethylpiperidin-4-yl 2,5-dimethylfuran-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Hydroxy-2,2,6,6-tetramethylpiperidine | HCID 75471 | — |
| 反応物 | 3-Furancarboxylic acid, 2,5-dimethyl-, methyl ester | HCID 80248 | — |
| 触媒 | Tetrabutoxytitanium | HCID 521701 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,2,6,6-Tetramethylpiperidin-4-yl 2,5-dimethylfuran-3-carboxylate | HCID 13765634 | — |
反応手順
154 g (1 mole) of methyl 2,5-dimethylfuran-3-carboxylate and 157 g (1 mole) of 4-hydroxy-2,2,6,6-tetramethylpiperidine were heated together with 10 g of tetrabutyl orthotitanate for 10 hours at about 190° C., the methanol formed being distilled off. When the reaction is complete, the mixture is cooled and the reaction mass is dissolved in ethyl acetate. The solution is extracted by shaking, first with 10% strength sodium carbonate solution and then with water, after which it is dried and evaporated down, and the residue is distilled under reduced pressure. The desired product distils at 142° C./2 mm as a virtually colorless oil which soon solidifies to a solid of melting point 59°-61° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04603205 |
| 出典データセット | uspto-grants-1986_07 |
| ORD ID | ord-66b19aa7576741619657092ed9d7f36e |
| 出典メモ | uspto-grants-1986_07 |