関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propionic Acid | HCID 1032 | — |
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 反応物 | 4,4,4-Trifluoro-3-methylbut-2-en-1-ol | HCID 54043180 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl 3-methyl-3-(trifluoromethyl)pent-4-enoate | HCID 10910798 | — |
反応手順
Triethyl orthoformate (6.51 mL, 35.7 mmol) was added to an ambient temperature mixture of 4,4,4-trifluoro-3-methylbut-2-en-1-ol (500 mg, 3.57 mmol) and propionic acid (13 μL, 0.18 mmol). After heating in a sealed tube at 200° C. for 30 h, the reaction mixture was cooled, diluted with diethyl ether and washed with saturated aqueous sodium bicarbonate. The organic phase was dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-20% ethyl acetate/hexane afforded ethyl 3-methyl-3-(trifluoromethyl)pent-4-enoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08106070B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-9b9a5bb07d734710b59aedda91ab7793 |
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| 出典メモ | uspto-grants-2012_01 |
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