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4-Aminophenol → 4-(2-Chloro-1,1-difluoroethoxy)benzeneamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminophenol | HCID 403 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Dichloro-1,1-difluoroethane | HCID 15442 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2-Chloro-1,1-difluoroethoxy)benzeneamine | HCID 19792700 | — |
反応手順
2.5 g (22.9 mmol) of p-aminophenol, 3.09 g (22.9 mmol) of 1,2-dichloro-1,1-difluoroethane, 5.48 g (39.6 mmol) of K2CO3 and 40 ml of dry acetonitrile were stirred together at room temperature for 5 days. The mixture was poured into water and extracted two times into ether. The combined ether extracts were washed with water, dried over MgSO4 and filtered: HCl gas was bubbled into the ether solution causing the above-named aniline to precipitate as the hydrochloride salt, which was collected by filtration and recrystallized twice from CH3CN to give 0.9 g (16 percent of theoretical d 245°-250° C.) of a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05250690 |
| 出典データセット | uspto-grants-1993_10 |
| ORD ID | ord-c511a8c8feb8478d9e51ff3b4f62f5c5 |
| 出典メモ | uspto-grants-1993_10 |