関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | Methyl 5-hexynoate | HCID 534077 | — |
| 反応物 | Methyl 3-acetamido-4-trifluoromethanesulfonyloxybenzoate | HCID 14493070 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 溶媒 | Diethylamine | HCID 8021 | — |
| 生成物 | Methyl 3-acetamido-4-(5-methoxycarbonyl-1-pentynyl)benzoate | HCID 22627137 | 86.5% |
反応手順
A mixture of methyl 3-acetamido-4-trifluoromethane-sulfonyloxybenzoate (1.43 g), methyl 5-hexynoate (582 mg), palladium(II) chloride (14 .9 mg), triphenylphosphine (43.8 mg) and cooper(I) chloride (32 mg) in diethylamine (18 ml) was stirred at 20° C. for 14 hours. The solvent was evaporated in vacuo an the residue was chromatographed on silica gel eluting with a mixture of hexane and ethyl acetate (1:2) to give methyl 3-acetamido-4-(5-methoxycarbonyl-1-pentynyl)-benzoate (1.15 g) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06358992B1 |
|---|
| 出典データセット | uspto-grants-2002_03 |
|---|
| ORD ID | ord-28b80c2cdc5a4419813945f88a1a28ba |
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| 出典メモ | uspto-grants-2002_03 |
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