化工社化工社 化学情報印刷レポート · 研究参考用
Sodium percarbonate → 3,4-Difluorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium percarbonate | HCID 159762 | — |
| 反応物 | 3,4-Difluorobenzophenone | HCID 569908 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 3,4-Difluorobenzoic acid | HCID 99166 | 95.5% |
反応手順
2.5 g of sodium percarbonate were added over 1 h to a solution of 2.2 g (10 mmol) of 3,4-difluorobenzophenone and 20 ml of trifluoroacetic acid (0° C.) and the temperature was then allowed to rise to 20° C. The mixture was stirred for 16 h at this temperature and 50 g of ice were then added. The mixture was subsequently extracted twice with dichloromethane and the organic phases were washed (NaHCO3) until the washings were neutral. The solvent was then removed. Working-up as described in Example 22 gave 1.2 g (7.6 mmol, 76%) of 3,4-difluorobenzoic acid, which can be obtained analytically pure from water (melting point 113°-120.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05481032 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-3a540bda32044b3891e823049d0d41e1 |
| 出典メモ | uspto-grants-1996_01 |