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Chloroform → Methyl 3-(1H-1,2,4-triazol-1-YL)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 1,3,5-Triazine | HCID 9262 | — |
| 反応物 | Methyl 3-hydrazinylbenzoate hydrochloride | HCID 23285088 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 3-(1H-1,2,4-triazol-1-YL)benzoate | HCID 22224836 | 76.7% |
反応手順
1.04 g of 1,3,5-triazine was added to a solution of 3.7 g of methyl 3-hydrazinobenzoate hydrochloride in 20 ml of ethanol. The mixture was refluxed by heating, for 3 hours. The reaction mixture was allowed to cool and mixed with chloroform. The resulting insolubles were removed by filtration. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluant: methylene chloride/methanol=100/0 to 100/1) and then subjected to crystallization from diisopropyl ether. The crystals were collected by filtration to obtain 2.0 g of methyl 3-(1,2,4-triazol-1-yl)benzoate as colorless needle-like crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06136826 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-4191be54d25d43f3805d5d3b5d35cb56 |
| 出典メモ | uspto-grants-2000_10 |