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Sulfuric Acid → 1,2,4-Triazolo(4,3-a)pyridin-3(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Chloropyridine | HCID 7977 | — |
| 反応物 | Glycol monoethyl ether | HCID 8076 | — |
| 反応物 | Semicarbazide hydrochloride | HCID 11236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,2,4-Triazolo(4,3-a)pyridin-3(2H)-one | HCID 81431 | 59% |
反応手順
A mixture of 50 g. (0.44 mole) of 2-chloropyridine and 98.22 g. (0.88 mole) of semicarbazide hydrochloride in 150 ml. of 2-ethoxyethanol was heated to reflux and then treated with a solution of 1 ml. of concentrated sulfuric acid (36 N) in 5 ml. of 2-ethoxyethanol. The resulting solution was refluxed for 18 hr., cooled to about 60°, and treated with 150 ml. of water. The mixture was stirred, cooled to 0°, and kept 0.5 hr. and the solid was collected on a filter. The solid was washed well with water and dried under reduced pressure, to give 35.0 g (59%) of product, m.p. 230°-231°, which was sufficiently pure to be used for the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04254124 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-3d13aa21801e4a6d9fde56452d9bf418 |
| 出典メモ | uspto-grants-1981_03 |