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Ethyl Acetoacetate → 6-Methyl-2-(3,4,5-trimethoxyphenylamino)-4(3H)pyrimidinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | HCID 178419082 | HCID 178419082 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Methyl-2-(3,4,5-trimethoxyphenylamino)-4(3H)pyrimidinone | HCID 136067274 | 49% |
反応手順
To a solution of sodium methoxide (0.96 g, 1.79 mmol) in methanol was added ethyl-3-oxo-butanoate (0.23 g, 1.79 mmol) and 3,4,5-trimethoxyphenylguanidinium nitrate (0.5 g, 1.79 mmol). The mixture was stirred at reflux for 17 h. The reaction mixture was cooled to room temperature and evaporated in vacuo to give a dark grey solid. Recrystallisation from ethanol gave the title compound (0.25 g, 49%) as a light grey solid, m.p. 228-230° (dec). δH (d6DMSO) 2.12 (3H, s), 3.61 (3H, s), 3.74 (6H, s), 5.69 (1H, s), 7.02 (2H, s), 8.70 (1H, br s) and 10.47 (1H, br s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05958935 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-1b0da2ee48d040c7bcd2d8820ff7cc5b |
| 出典メモ | uspto-grants-1999_09 |