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Water → Methyl 4-(3-hydroxyprop-1-ynyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Propargyl alcohol | HCID 7859 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 4-iodobenzoate | HCID 69273 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 4-(3-hydroxyprop-1-ynyl)benzoate | HCID 4448596 | 87.5% |
反応手順
To a solution of methyl 4-iodobenzoate (20 g, 76 mmol), propargyl alcohol (5.55 g, 99.0 mmol) and triethylamine (20 mL) in acetonitrile (200 mL) was added dichlorobis(triphenylphosphine)palladium(II) (1.55 g, 2.21 mmol), followed by Cul (454 mg, 2.38 mmol). The reaction mixture was stirred at room temperature for 24 h. Water was added and the aqueous solution was washed with EtOAc (3×). The organic solutions were combined, dried (MgSO4), filtered and concentrated. Purification by medium pressure chromatography (9:1 hexanes:EtOAc to 4:1 hexanes:EtOAc) provided 4-(3-hydroxy-prop-1-ynyl)-benzoic acid methyl ester (12.65 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07192979B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-0357100c33974090aafecf3d49ce4352 |
| 出典メモ | uspto-grants-2007_03 |