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Water → 1-[2-(4-Phenoxyphenoxy)ethyl]pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 4-Phenoxyphenol | HCID 13254 | — |
| 反応物 | 1-(2-Chloroethyl)pyrrolidine hydrochloride | HCID 81668 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[2-(4-Phenoxyphenoxy)ethyl]pyrrolidine | HCID 9993978 | 92.9% |
反応手順
A solution of 4-phenoxyphenol (0.56 g, 3.0 mmol), 1-(2-chloroethyl)-pyrrolidine HCl (0.51 g, 3.0 mmol) and powdered K2 CO3 (1.2 g, 8.7 mmol) in 30 mL DMF was stirred at 80°-90° C. for 15 hours. The solution was cooled, poured into Et2O and water and the ether layer washed with water and brine, dried over Na2SO4 and concentrated in vacuo to give 0.79 g of a brown oil. The crude product was flashed chromatographed on silica gel using a gradient of 2:1 hexane/EtOAc to 100% EtOAc to provide the title compound (0.65 g, 76.5%) as a light yellow oil:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05719306 |
| 出典データセット | uspto-grants-1998_02 |
| ORD ID | ord-f93b476cf09347448a0e0dc2dd20eee4 |
| 出典メモ | uspto-grants-1998_02 |