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Hydrogen Peroxide → 2-Chloro-4,5-difluorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | (2-Chloro-4,5-difluorophenyl)(phenyl)methanone | HCID 704945 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2-Chloro-4,5-difluorobenzoic acid | HCID 737171 | 88% |
反応手順
32 g of 20% hydrogen peroxide solution are added dropwise over 30 min to a solution of 37.8 g (0.15 mol) of 2-chloro-4,5-difluorobenzophenone in 400 g of 100% sulfuric acid in such a way that the temperature remains below 35° C. The reaction is complete after 7 h. The reaction mixture is then poured on to 1200 g of ice. Extraction of the mother liquor with methyl tert-butyl ether, isolation of the crude product from the extract and crystallization from water gives 17.0 g (0.0883 mol, 88%) of colorless 2-chloro-4,5-difluorobenzoic acid melting at 104.4°-105.8° 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-8cd1f6bc4278422bb9c35eef57c43084 |
| 出典メモ | uspto-grants-1996_01 |