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Sulfuric Acid → 3-(3,5-Difluorophenyl)propionic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3-(3,5-Difluorophenyl)acrylic acid | HCID 522810 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(3,5-Difluorophenyl)propionic acid | HCID 3669498 | 92.2% |
反応手順
Hydrogenate a mixture of 3,5-difluorocinnamic acid (10.0 g, 54.3 mmol), 5% palladium on carbon (1.5 g), and concentrated sulfuric acid (10 ml) in tetrahydrofuran (195 ml) at 60 psi at room temperature overnight. After filtering the catalyst, dilute with ether, wash with water twice, dry over anhydrous sodium sulfate, and concentrate to obtain the title compound as clear colorless crystals (9.32 g, 92%). NMR (400 MHz, CDCl3): δ 2.67 (t, 2H), 2.94 (t, 2H), 6.65 (t, 1H), 6.74 (d, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728150B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-53d1feeb0cf9479f8fdc097813fafe67 |
| 出典メモ | uspto-grants-2010_06 |