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4-Oxo-4-(4'-trifluoromethyl-biphenyl-4-yl)-butyric acid, methyl ester → 4-Oxo-4-(4'-trifluoromethyl-biphenyl-4-yl)-butyric acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Oxo-4-(4'-trifluoromethyl-biphenyl-4-yl)-butyric acid, methyl ester | HCID 12056884 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4-Oxo-4-(4'-trifluoromethyl-biphenyl-4-yl)-butyric acid | HCID 23005240 | 99% |
反応手順
In a manner similar to Example 4, Step (b), 4-oxo-4-(4′-trifluoromethyl-biphenyl-4-yl)-butyric acid, methyl ester (1.34 g, 0.00398 mol) was refluxed in 6 M aqueous hydrochloric acid (24 mL) to give 1.27 g of 4-oxo-4-(4′-trifluoromethyl-biphenyl-4-yl)-butyric acid as an 80% pure solid. A portion (0.059 g) of the material was purified by chromatography on silica gel (7 g, 230-400 mesh), eluting with dichloromethane (15×10 mL); dichloromethane-methanol (15:1, 16×10 mL) to give 0.0476 g of pure 4-oxo-4-(4′-trifluoromethyl-biphenyl-4-yl)-butyric acid as an off-white solid; mp 172-174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06307089B2 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-d6b132eeb3d74158aa10539681ea7bce |
| 出典メモ | uspto-grants-2001_10 |