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Sodium Carbonate → 1-[3-Methoxy-5-(trifluoromethyl)phenyl]pyrrolidin-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,4-Dibromo-2-butanol | HCID 29570 | — |
| 反応物 | 5-(Trifluoromethyl)-m-anisidine | HCID 605671 | — |
| 生成物 | 1-[3-Methoxy-5-(trifluoromethyl)phenyl]pyrrolidin-3-ol | HCID 67022283 | 47% |
反応手順
3-Methoxy-5-(trifluoromethyl)aniline (15.0 g) and 1,4-dibromobutan-2-ol (18.3 g) were stirred at 100° C. for 3 hr. After cooling to room temperature, to the reaction mixture was added saturated aqueous sodium carbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate 90:10-50:50) to give the title compound (9.57 g, yield 47%) as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08338622B2 |
| 出典データセット | uspto-grants-2012_12 |
| ORD ID | ord-3ccd6a71f3a2457f9a639a45b543f266 |
| 出典メモ | uspto-grants-2012_12 |