反应详情

温度

0 °C

7.0 g (33.8 mmol) of 3-cyclopentyloxy-4-methoxy-phenylamine (Garcia et al., JOC, 2005, 70, p 1050) were dissolved in 150 ml of DCM. The solution was cooled to 0° C. and 5.74 g (40.5 mmol) isonicotinoyl chloride in 50 ml DCM were added to the solution. A precipitate was formed. The reaction mixture was subsequently stirred at room temperature during two hours. A solution of 2.7 g NaOH in 100 ml water was added to the reddish reaction mixture. The organic layer was separated, dried over Na2SO4 and evaporated. The crude product was purified by flash chromatography on silica gel (ethyl acetate/n-hexane 2:1) to afford 7.2 g (62%) of the desired product. MS (ESI): 313.1.

1. customA precipitate was formed
2. customThe organic layer was separated
3. dry with materialdried over Na2SO4
4. customevaporated
5. customThe crude product was purified by flash chromatography on silica gel (ethyl acetate/n-hexane 2:1)