関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | (5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol | HCID 17862912 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-(Bromomethyl)-5-chloro-1-phenyl-3-(trifluoromethyl)-1H-pyrazole | HCID 17862890 | 279% |
反応手順
A solution of 3.0 g (10.9 mmoles) of (5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol dissolved in 60 ml of diethyl ether was cooled to −10° C. Thereto was added 1.0 g (3.8 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 1 hour to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 3.6 g (yield: 95.8%) of 4-bromomethyl-5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazole as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07238689B2 |
|---|
| 出典データセット | uspto-grants-2007_07 |
|---|
| ORD ID | ord-c24130dac1174430bcddebccd9a772ee |
|---|
| 出典メモ | uspto-grants-2007_07 |
|---|