関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine-4-amidine hydrochloride | HCID 2776844 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 3,3-Dimethoxy-2-methoxycarbonylpropen-1-ol | HCID 59117939 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 2-(pyridin-4-yl)pyrimidine-5-carboxylate | HCID 69122655 | 88% |
反応手順
To a solution of isonicotinamidine hydrochloride (1 g, 6.35 mmol) in anhydrous DMF (12 mL) is added sodium salt of 2-dimethoxymethyl-3-hydroxy-acrylic acid methyl ester (1.46 g, 7.36 mmol) and the reaction mixture is heated at 100° C. under nitrogen for 1 h. The reaction is cooled to room temperature and water (48 mL) is added. The precipitate is collected by filtration, washed with water and vacuum dried to afford 2-pyridin-4-yl-pyrimidine-5-carboxylic acid methyl ester (1.2 g, 88%). MS: 216 (M+H); 1H NMR (300 MHz, CD3OD): δ 4.00 (s, 3H), 8.44 (d, 2H), 8.73 (d, 2H), 9.38 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08202863B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-9dc033b50dac4503bb2dff46aff4e7db |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|
