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Phosphoric Acid → 1,1-Dimethylprop-2-ynyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Methyl-3-butyn-2-ol | HCID 8258 | — |
| 触媒 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,1-Dimethylprop-2-ynyl acetate | HCID 74144 | — |
反応手順
112 g (one mole) of freshly distilled dimethylethynyl carbinol is treated with 1.2 moles of acetic anhydride containing 10 drops of 85% phosphoric acid. The acetic anhydride is added to the carbinol dropwise with shaking while maintaining the temperature under 40°. The mixture is allowed to stand overnight, washed with two 75 ml portions of cold water, and the water washings are extracted with ether. The ether extract is added to the main portion of ester and the combined ethereal solution is washed with 10% sodium carbonate solution until the washings remain basic to litmus. The solution is washed with two 75 ml portions of ice-water, dried over calcium chloride, and distilled to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04179561 |
| 出典データセット | uspto-grants-1979_12 |
| ORD ID | ord-eeb4d768e0df41d28f5e39b4c5ee9d53 |
| 出典メモ | uspto-grants-1979_12 |