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Methanol → 4,6-Dimethoxypyrimidine-5-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4,6-Dichloro-5-pyrimidinecarbaldehyde | HCID 819691 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 生成物 | 4,6-Dimethoxypyrimidine-5-carbaldehyde | HCID 4436645 | 20% |
反応手順
43.6 g (246 mmol) of 4,6-dichloropyrimidine-5-carboaldehyde was dissolved in 200 ml of methanol, and 120 g (622 mmol) of 28% sodium methoxide was added under cooling with ice and then reacted for 2 hours at room temperature. After completion of the reaction, the solvent was distilled off, and an aqueous citric acid solution was added, followed by extraction with ethyl acetate. The organic layer was washed with an aqueous sodium hydrogencarbonate solution, an aqueous citric acid solution, water and an aqueous sodium chloride solution in this order, dried and concentrated, and the obtained crude crystals were washed with isopropyl ether to obtain 8.3 g (yield: 20%) of 4,6-dimethoxypyrimidine-5-carboaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06806230B1 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-3365243bc67640c2b8828e7859d2fbfe |
| 出典メモ | uspto-grants-2004_10 |