関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Pyrimidine-5-carboxaldehyde | HCID 2761034 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | N-(5-pyrimidinylmethyl)ethylenediamine | HCID 13910892 | 84.8% |
反応手順
Ethylenediamine (60 g) was dissolved in benzene (200 ml), and 5-formylpyrimidine (21.6 g) was added at room temperature. Subsequently, the mixture was heated, and refluxed for 3 hours while removing water as an azeotrope. After the reaction, benzene and the excess of ethylenediamine were distilled off under reduced pressure. The residue was dissolved in ethanol (200 ml). Sodium borohydride (8.4 g) was added portionwise to this solution at room temperature, and subsequently the mixture was stirred at room temperature for 5 hours. Ethanol was distilled off under reduced pressure. Dichloromethane (100 ml) was added to the residue, and a dichloromethane-soluble portion was separated. Dichloromethane was distilled off from the dichloromethane layer under reduced pressure to give N-(5-pyrimidinylmethyl)ethylenediamine (25.8 g) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05428032 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-27d3f817215040c68e8c00bc79b7b9f9 |
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| 出典メモ | uspto-grants-1995_06 |
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