関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | alpha-(1-Chlorocyclopropyl)-alpha-((2-chlorophenyl)methyl)-1H-1,2,4-triazole-1-ethanol | HCID 119361 | — |
| 反応物 | Sulfur | HCID 5362487 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | HCID 178520209 | HCID 178520209 | 93% |
反応手順
A mixture of 3.12 g (10 mmol) of 2-(1-chloro-cyclopropyl)-1-(2-chlorophenyl)-3-(1,2,4-triazol-1-yl)-propan-2-ol and 45 ml of absolute tetrahydrofuran is treated at 20° C. with 8.4 ml (21 mmol) of n-butyl-lithium in hexane, and the mixture is stirred at 0° C. for 30 minutes. The reaction mixture is then cooled to -70° C., 0.32 g (10 mmol) of sulphur powder are added, and the mixture is stirred for 30 minutes at -70° C. It is heated to -10° C., and treated with ice-water and brought to a pH of 5 by adding dilute sulphuric acid. The mixture is extracted repeatedly using ethyl acetate, and the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. In this manner, 3.2 g (93% of theory) of 2-(1-chloro-cyclopropyl)-1-(2-chlorophenyl)-3-(5-mercapto-1,2,4-triazol-1-yl)-propan-2-ol are obtained in the form of a solid which, after recrystallization, melts at 138°-139° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05789430 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-28423d9f0c2c4de4ba935d927efcac61 |
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| 出典メモ | uspto-grants-1998_08 |
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