反应详情

温度

125 °C

To a stirred solution of N-(4,6-dichloropyridin-3-yl)-N2-(3-methylbutyl)alaninamide (350 mg, 1.15 mmol) in DMF (1.0 mL) was added tri-basic potassium phosphate (250 mg, 1.20 mmol). The reaction mixture was heated to 125° C. and stirred at the same temperature for 3 h. The reaction was then cooled to rt, diluted with water (5 mL) and the aqueous phase was extracted with ethyl acetate (25 mL×3). The combined organic phases were washed with water, dried over Na2SO4 and evaporated to give desired product (Yield: 33%), which was used for next step without any further purifications. 1HNMR (CDCl3, 300 MHz) δ 0.90-1.01 (m, 6H), 1.33 (d, 3H), 1.52-1.75 (m, 2H), 1.80 (s, 1H), 3.10-3.19 (m, 1H), 3.31-3.42 (m, 1H), 4.07 (q, 1H), 6.51 (s, 1H), 7.65 (s, 1H), 9.41 (br s, 1H).

1. temperatureThe reaction was then cooled to rt
2. extractionthe aqueous phase was extracted with ethyl acetate (25 mL×3)
3. washThe combined organic phases were washed with water
4. dry with materialdried over Na2SO4
5. customevaporated