化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 1-Trimethylsilyl-1,2,4-triazole | HCID 87558 | — |
| 反応物 | 2-(2,4-Difluorophenyl)-2-methyloxirane | HCID 19708648 | — |
| 反応物 | HCID 178507090 | HCID 178507090 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane | HCID 15516903 | — |
反応手順
5.13 g (0.03 moles) of 1,2-epoxy-2-(2,4-difluorophenyl)-propane are reacted with 6.35 g (0.045 moles) of 1-(trimethylsilyl)-1,2,4-triazole and 0.14 g (0.0015 moles) of 1,2,4-triazol-1-yl sodium in 40 ml of dimethyl formamide at 80° C. for 3 hours. Then the reaction mixture is cooled to room temperature, neutralized by glacial acetic acid, mixed with 200 ml of water and extracted twice with 50 ml of dichloromethane each. The combined extracts are washed three times with 50 ml of water each, dried over water-free sodium sulfate and evaporated in vacuo. After carrying out a separation as described in Example 5, removal of the solvent and crystallization from n-heptane 6.0 g (64.5%) of the title compound are obtained; m.p.: 51°-53° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05707976 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-f1cd7047a8394a479c696b57110fd9b6 |
| 出典メモ | uspto-grants-1998_01 |