関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4-Amino-2-methyl-5-pyrimidinemethanamine | HCID 66762 | — |
| 生成物 | 2-Methyl-4-amino-5-aminomethylpyrimidine carbonate | HCID 17991879 | — |
反応手順
A solution of 50 g of crude 2-methyl-4-amino-5-aminomethylpyrimidine (purity: 95.0%, 0.344 mole) dissolved in 250 g of methanol was charged into a four-necked flask equipped with a stirrer, an introducing tube for carbon dioxide, a reflux condenser and a thermometer, followed by maintaining the temperature of the solution at 20° C. Subsequently, 64 g (1.45 mole) of carbon dioxide was blown into the solution over about one hour and the reaction was carried out to precipitate a white crystal of a 2-methyl-4-amino-5-aminomethylpyrimidine carbonate with extreme easiness. Then, the resulting crystal was filtered off, washed with a small amount of methanol, and dried at 20° C. until it may have constant weight to give 61.8 g of 2-methyl-4-amino-5-aminomethylpyrimidine carbonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04892948 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-894f3bfc968d4d229dc5c7495ba79859 |
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| 出典メモ | uspto-grants-1990_01 |
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