関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,4,6-Triaminopyrimidine | HCID 13863 | — |
| 反応物 | Nitromalonaldehyde | HCID 313475 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Nitropyrido[2,3-d]pyrimidine-2,4-diamine | HCID 11052776 | — |
反応手順
About 1 equivalent of 2,4,6-triamino pyrimidine was suspended in about 50 ml of refluxing absolute ethanol with stirring under an atmosphere of nitrogen. Concentrated HCl was added dropwise to effect solution and as soon as solution occurred, about 1.2 equivalents of nitromalonaldehyde was added all at once. Within 10 minutes, a thick reddish voluminous precipitate started forming. TLC analysis indicated the presence of a yellow spot corresponding to that of the desired product along with staring materials. The reaction mixture was stirred at reflux for 3.5 hours, immediately diluted with 30 ml of water, cooled and neutralized with concentrated NH4OH. The precipitate was collected on a funnel and was washed repeatedly with water to remove unreacted triamino pyrimidine to yield pure 2,4-diamino-6-nitropyrido[2,3-d]pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06103727 |
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| 出典データセット | uspto-grants-2000_08 |
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| ORD ID | ord-4b2993cec67f453f813a5db2757fd05f |
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| 出典メモ | uspto-grants-2000_08 |
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