反应详情

温度

80 °C

A solution of N-allyl, N-trifluoroacetyl-1-(2-iodo-5-methoxyphenyl)-2-propylamine (4.45 g, 10.8 mmol) in dimethylformamide (120 mL) was treated with KOAc (3.17 g, 32.3 mmol), n-Bu4NBr (3.47 g, 10.8 mmol), PPh3 (0.283 g, 1.08 mmol), Pd(OAc)2 (0.242 g, 1.08 mmol) and stirred overnight at 80° C. The product mixture was cooled to 20° C., filtered, diluted with water (200 mL), extracted with ether (3×200 mL), the combined organic phases washed with water (100 mL), brine (100 mL), dried with Na2SO4 and concentrated. Flash chromatography (10% EtOAc in hexane, silica) resulted in 1.39 g of a yellow oil.

1. temperatureThe product mixture was cooled to 20° C.
2. filtrationfiltered
3. additiondiluted with water (200 mL)
4. extractionextracted with ether (3×200 mL)
5. washthe combined organic phases washed with water (100 mL), brine (100 mL)
6. dry with materialdried with Na2SO4
7. concentrationconcentrated