関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Hydroxyisovaleric acid | HCID 69362 | — |
| 反応物 | Hydrochloride methanol | HCID 21893726 | — |
| 生成物 | Methyl 3-hydroxy-3-methylbutanoate | HCID 521979 | — |
反応手順
In 50 ml of 7 wt. % hydrochloric acid methanol solution was dissolved 1.18 g of β-hydroxyisovaleric acid, and an reaction was allowed to proceed at room temperature overnight. The solvent was removed from the solution as reacted by distillation under a reduced pressure to obtain 1.30 g of crude methyl β-hydroxyisovalerate. The crude methyl β-hydroxyisovalerate was dissolved in diethyl ether, and 0.91 g of 3,4-dihydro-2H-pyran and a catalytic amount of p-toluenesulfonic acid were added thereto. Stirring was continued at room temperature overnight for reaction. The resultant reaction mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate and then with water and dried over magnesium sulfate. The solvent was removed from the dried reaction mixture by distillation under a reduced pressure to obtain 1.98 g of crude methyl β-dihydropyranyloxyisovalerate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05480580 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-5c480e0b8a754195a1ecb4a2cbff6a4a |
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| 出典メモ | uspto-grants-1996_01 |
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