関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acrylate | HCID 8821 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2-Iodo-6-methylpyridin-3-ol | HCID 89957 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 触媒 | Palladium Chloride | HCID 24290 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl (3-hydroxy-6-methylpyridin-2-yl)propenoate | HCID 131720091 | — |
反応手順
To a solution of 3-hydroxy-2-iodo-6-methylpyridine (1.175 g, 5.0 mmol) in DMF (9.5 ml) and water (0.5 ml) were added potassium acetate (1.23 g, 12.5 mmol), triphenylphosphine (105 mg, 0.40 mmol), palladium chloride (36 mg, 0.20 mmol) and ethyl acrylate (1.63 ml, 1.50 g, 15.0 mmol). The mixture was placed under nitrogen and heated at 120° C. for 1.5 h. The mixture was cooled, filtered from deposited palladium black, and added to water (100 ml). The product was extracted into ethyl acetate (3×30 ml). The combined extracts were washed with water (2×25 ml) and with brine (25 ml), then dried over sodium sulphate and evaporated. This left a tan solid, the product (951 mg, 91%). mp 192°-195° C. (dec)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05726315 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-daea2679130c4e96a69efc91647c4537 |
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| 出典メモ | uspto-grants-1998_03 |
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