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1-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one → 7-(3-Pyridinyl)[1,2,4]triazolo[1,5-a]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one | HCID 567033 | — |
| 反応物 | HCID 178418311 | HCID 178418311 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 7-(3-Pyridinyl)[1,2,4]triazolo[1,5-a]pyrimidine | HCID 900944 | — |
反応手順
A mixture of 2.54 g of 3-amino-1,2,4-triazole, 5.29 g of 3-dimethylamino-1-(3-pyridyl)-2-propene-1-one and 25 ml of glacial acetic acid was heated under reflux for 6 hours. The solvent was removed in vacuo and the solid residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane. The organic layer was separated and dried over powdered anhydrous sodium sulfate. This solution was passed through a short column of a hydrous magnesium silicate and the effluent was refluxed on a steam bath with the gradual addition of hexane until crystallization was noted. On cooling the desired compound was separated and collection by filtration gave 1.95 g. of colorless crystals mp. 209°-210° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04444774 |
| 出典データセット | uspto-grants-1984_04 |
| ORD ID | ord-71b0cc88388149b8b5c31ae457814789 |
| 出典メモ | uspto-grants-1984_04 |