関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 反応物 | 2-tert-Butyl-2-[(4-chlorophenoxy)methyl]oxirane | HCID 12763621 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | alpha-((4-Chlorophenoxy)methyl)-alpha-(1,1-dimethylethyl)-1H-1,2,4-triazole-1-ethanol | HCID 123676 | 65% |
反応手順
72.15 g (0.3 mole) of 2-(4-chlorophenoxy-methyl)-2-tert.-butyl-oxirane and 24.15 g (0.35 mole) of 1,2,4-triazole were heated under reflux in 120 ml of ethanol for 48 hours. The mixture was then concentrated, the residue was taken up in 200 ml of ethyl acetate and the ethyl acetate mixture was heated. It was then cooled in an ice bath and the solid was filtered off and rinsed with ethyl acetate. The filtrate was concentrated, the residue was dissolved in ether/hexane and the solution was gassed with hydrogen chloride. The precipitate was filtered off and rinsed with ether and the free base was obtained by adding ethyl acetate/1N sodium hydroxide solution. 60.2 g (65% of theory) of 2-(4-chlorophenoxy-methyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 84°-87° C. were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04897107 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-37d0373e89ea449f84c8f278c252e002 |
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| 出典メモ | uspto-grants-1990_01 |
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