関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Octafluorotoluene | HCID 9906 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 反応物 | HCID 23672351 | HCID 23672351 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-Benzyloxycarbonylphenoxy)-1-trifluoromethyl-3,4,5,6-tetrafluorobenzene | HCID 18459336 | 95% |
反応手順
35.4 g of octafluorotoluene (0.15 mol) are dissolved in 400 ml of dimethylformamide, the solution is cooled to 0° C. using a cryostat, and a solution of 40 g of potassium 4-benzyloxycarbonylphenoxide (0.15 mol) in 300 ml of dimethylformamide is then added drop wise over the course of 2 hours. After 24 hours at 0° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, the residue is taken up in a little tetrahydrofuran, and the solution is filtered through a silica-gel column. The clear solution obtained is evaporated in a rotary evaporator until the reaction product precipitates out. The reaction product is then stirred in n-hexane, filtered off through a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06310238B1 |
|---|
| 出典データセット | uspto-grants-2001_10 |
|---|
| ORD ID | ord-abc300a4da914b51b691bb5f59f57a8d |
|---|
| 出典メモ | uspto-grants-2001_10 |
|---|