関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 3,5-diallyloxyphenylacetate | HCID 23116191 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | Methyl 2-acetyl-3,5-diallyloxyphenylacetate | HCID 68421776 | 70.4% |
反応手順
Methyl 3,5-diallyloxyphenylacetate (40 g, 0.14 mol) obtained in Example 5, Step 1 was dissolved in trifluoroacetic acid (0.15 L). After the solution was cooled to 4° C., acetic acid (9.5 mL, 0.17 mol) and trifluoroacetic anhydride (40 mL, 0.28 mol) were added thereto, followed by stirring at 4° C. for 3.5 hours. The reaction mixture was gradually added to a saturated aqueous solution of sodium hydrogencarbonate for neutralization, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/20-1/6) to obtain methyl 2-acetyl-3,5-diallyloxyphenylacetate (30 g, 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07767693B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-7e45bf1e3f5e448c849e1aa7fa713d8f |
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| 出典メモ | uspto-grants-2010_08 |
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