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Thionyl Chloride → HCID 178509687、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | HCID 178509718 | HCID 178509718 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178509687 | HCID 178509687 | 31.2% |
反応手順
7.21 g of crude 4-[1-hydroxycyclopent-1-yl-1-(1,2,4-triazolyl) methyl]benzonitrile is dissolved in 50 ml of dichloromethane at 0° and stirred at 0° with 24 ml of thionyl chloride for 1 hour. Then the mixture is concentrated to dryness under vacuum, dissolved in 50 ml of dichloromethane, stirred for 2 hours with 32 ml of triethylamine, diluted with water, extracted four times with ethyl acetate, washed with sodium chloride solution, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, thus obtaining 2.1 g of 4-[1-cyclopentylidene-1- (1,2,4triazolyl)methyl]benzonitrile as the free base, mp 72°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411982 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-1832dcb6f4e94f8cb76c4ac0847ee3d7 |
| 出典メモ | uspto-grants-1995_05 |