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Acetonitrile → 1-[2-[Bis(4-fluorophenyl)methoxy]ethyl]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 1-[Bis(4-fluorophenyl)methoxy]-2-chloroethane | HCID 10779302 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-[2-[Bis(4-fluorophenyl)methoxy]ethyl]pyrrolidine | HCID 827316 | 48% |
反応手順
1-[Bis(4-fluorophenyl)methoxy]-2-chloroethane (3) (0.92 g, 3.3 mmol) was added to acetonitrile (50 ml) containing potassium carbonate (1.1 g, 8.0 mmol). This was followed by the addition of pyrrolidine (0.51 g, 7.2 mmol). The resulting mixture was then heated to reflux for 72 hours under an atmosphere of nitrogen. At the end of this time, the solution was added to ether (75 ml), washed with water (50 ml) and brine (50 ml). This was then dried over anhydrous magnesium sulfate, filtered and evaporated at reduced pressure to give a clear light yellow oil. The oil was chromatographed on silica gel and eluted with 3:1 ethyl acetate/methanol to afford the desired product (4) (500 mg, 48%) as a clear light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05747523 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-e46e307586d74e3889ff99bf33479c04 |
| 出典メモ | uspto-grants-1998_05 |