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Water → 5-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Benzoylacetone | HCID 7166 | — |
| 反応物 | 3,5-Diamino-1,2,4-triazole | HCID 15078 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amine | HCID 975713 | 100% |
反応手順
A mixture of 7.0 g (71 mmol) 3,5-diamino-1,2,4-triazole and 12.0 g (74 mmol) benzoylacetone in 100 ml of glacial acetic acid was heated at reflux 2 hours. After cooling, methylene chloride (200 ml) was added followed by the addition of excess water. The organic layer was separated, washed with water, brine, dried over magensium sulfate and evaporated in vacuo to give a solid residue to which ethyl acetate was added. Filtering gave 16.0 g of crude 5-methyl-7-phenyl-1,2,4-triazolo[1,5-a]pyrimidin-2-amine (m.p. 246°-250° C.) which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05127936 |
| 出典データセット | uspto-grants-1992_07 |
| ORD ID | ord-d978f1943c9f42c9a878a6ac2d50f561 |
| 出典メモ | uspto-grants-1992_07 |