関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Acrylate | HCID 7294 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Bromopyridine | HCID 14268 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Pyridin-4-YL-acrylic acid methyl ester | HCID 98163 | 93,152.5% |
反応手順
A mixture of 4-bromopyridine (40.6 g, 0.25 mmol), palladium acetate (1.16 g, 5.14 mmol), tri-(O-tolyl)phosphine (3.14 g, 10.3 mmol), CH3CN (129 mL), triethylamine (64.3 mL, 0.46 mmol) and methyl acrylate (46.8 mL, 0.514 mmol) was sealed in a bomb and placed in an oil bath at 120° C. for 4 hours. The mixture was cooled to 0° C., the bomb was vented, and the slurry thus obtained was partitioned between CH2Cl2 /water. The aqueous phase was separated, extracted with CH2Cl2 (2×200 mL) and the combined organic layers were dried over MgSO4. The solvent was removed in vacuo to afford 38 g of methyl 3-(4-pyridyl)propenoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05624922 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-36f848040a24470e840b0595554b77fa |
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| 出典メモ | uspto-grants-1997_04 |
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