関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetamidine monohydrochloride | HCID 67170 | — |
| 反応物 | 4-(Dimethylamino)-1,1-dimethoxybut-3-en-2-one | HCID 2782145 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(Dimethoxymethyl)-2-methylpyrimidine | HCID 2799572 | 91.3% |
反応手順
Acetamidine hydrochloride (3 mol) and 4-dimethylamino-1,1-dimethoxy-but-3-en-2-one (2 mol) were mixed in methanol (500 ml) and the reaction mixture was warmed to 40° C. A solution of sodium methoxide in methanol (558 g, 30%) was added quickly and a brown suspension was formed. The reaction mixture was heated under reflux for 2 h, cooled to room temperature overnight followed by evaporation of methanol under reduced pressure. The resulting residue was taken up in dichloromethane (500 ml) and washed several times with water (100 mL). The solvent was removed to give 307 g of black oil. The distillation of this oil gave a colourless liquid of boiling point 55-58° C. (0.5 mbar).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08178540B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-e4f679468da6435e90e93b8b381cd5bc |
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| 出典メモ | uspto-grants-2012_05 |
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