反应详情

温度

50 °C

620 mg of 2-phenoxyethanimidamide hydrochloride (0.00333 mol) are desalified in dichloromethane by the action of a 3N sodium hydroxide solution. After decantation and extraction of the aqueous phase by dichloromethane, the organic phase is dried over sodium sulphate then evaporated to dryness. The white powder obtained is solubilized in dimethylformamide (30 ml). 275 mg of 2-bromo-1-[4-(4-fluorophenoxy)phenyl]propan-1-one (0.000851 mol) is added. The mixture is heated at 50° C. for 20 hours then returned to 23° C. before adding 25 ml of water and 30 ml of ethyl acetate. After extraction with ethyl acetate, the organic phase is dried over sodium sulphate then evaporated in a rotary evaporator under vacuum. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 2-8). A pale yellow-coloured foam is obtained.

1. extractionAfter decantation and extraction of the aqueous phase by dichloromethane
2. dry with materialthe organic phase is dried over sodium sulphate
3. customthen evaporated to dryness
4. customThe white powder obtained
5. customthen returned to 23° C.
6. extractionAfter extraction with ethyl acetate
7. dry with materialthe organic phase is dried over sodium sulphate
8. customthen evaporated in a rotary evaporator under vacuum
9. customThe residue obtained
10. customthen purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 2-8)
11. customA pale yellow-coloured foam is obtained