関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(4-Chlorobenzyl)-3,3-dimethyl-2-hydroxy-2-methylsulphonyloxymethylcyclopentane | HCID 14721906 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | Metconazole | HCID 86210 | — |
反応手順
A mixture of 0.22 g 1-(4-chlorobenzyl)-3,3-dimethyl-2-hydroxy-2-methylsulphonyloxymethylcyclopentane prepared as described in Example 1 (j), 47 mg 1,2,4-triazole and 0.1 g potassium carbonate in 3 ml N-methylpyrrolidone was warmed at 50° C. for 2 hours. A further 0.1 g potassium carbonate was then added, the temperature was raised to 120° C. and the reaction continued overnight at this temperature. The reaction mixture was then partitioned between diethyl ether and water and the organic solution flashed to give 1-(4-chlorobenzyl)-3,3-dimethyl-2-hydroxy-2-(1,2,4-triazol-1-yl)methylcyclopentane crystallised from petroleum as a single stereoisomer (Isomer A). The conversion yield of Isomer A, corrected for purity, was 72%. The structure of the product was established by n.m.r. spectroscopy. Purity of Isomer A was 90% and Isomer B was not detected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05262543 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-142949d75c8f4b58905fc73b4b785d3e |
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| 出典メモ | uspto-grants-1993_11 |
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