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Chlorohydroquinone → Phenylpropynoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorohydroquinone | HCID 301 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Phenylacetylene | HCID 10821 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 生成物 | Phenylpropynoic acid methyl ester | HCID 138378 | — |
反応手順
A solution of phenylacetylene (10, 2 mmol), chlorohydroquinone(HQ-Cl) (0.4 mmol), molybdovanadophosphate (NPMoV) (35 mg) and palladium (II) acetate (50 mg) in methanol (10 mL) is stirred under CO/O2 (10 atm/0.5 atm) at 25° C. for 15 h. The reaction is then quenched with wet ether and the product is extracted with n-hexane. After removal of the solvent under reduced pressure, the product is isolated by column chromatography over silica gel (hexane:ethyl acetate 5:1) to give pure methyl phenylpropiolate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06579988B2 |
| 出典データセット | uspto-grants-2003_06 |
| ORD ID | ord-6c1949234d864167946a004a2d2318f4 |
| 出典メモ | uspto-grants-2003_06 |