関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2,4-Dichloro-4',5-difluorobenzophenone | HCID 18997590 | — |
| 溶媒 | Fuming sulfuric acid | HCID 24681 | — |
| 生成物 | 2,4-Dichloro-5-fluorobenzoic acid | HCID 688138 | — |
反応手順
28.7 g (0.1 mol) of 2,4-dichloro-4',5-difluorobenzophenone are dissolved in 250 g of 10% oleum, and 25 g of 50% hydrogen peroxide solution are added at temperatures up to 30° C. When the metered addition has ended (30 min), the mixture is heated for 8 h at 50° C. and, after cooling, is poured on to 250 g of ice. This mixture is kept for 8 h at 140° C. and 4-fluorophenol is then recovered by steam distillation (7.5 g, 0.0673 mol, 67%, m.p. (DSC) 42.6° C.). 2,4-dichloro-5-fluorobenzoic acid is isolated as described in Example 1 (17.0 g, 0.0813 mol, 81%, m.p. 143°-145° C.). (DSC =differential scanning calorimetry)
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-92edf459b2944c84a9abcea8d2cc2943 |
|---|
| 出典メモ | uspto-grants-1996_01 |
|---|