反应详情

Ethyl isonipecotate (6.0 g, 38.66 mmol), 4-chloropyridine hydrochloride (5.9 g, 38.66 mmol) and N-methylmorpholine (9.3 mL, 85.0 mmol) were dissolved in N-methylpyrrolidinone (50 mL) and the resulting solution heated at 100° for 48 h. The solution was concentrated in vacuo and the residue dissolved in ethyl acetate (200 mL), washed with water and brine (2×100 mL), then dried (Na2SO4) and evaporated. The resulting residue was purified by flash chromatography (5%MeOH/CH2Cl2) to afford 21-1 as a crystalline solid.

1. temperaturethe resulting solution heated at 100° for 48 h
2. concentrationThe solution was concentrated in vacuo
3. dissolutionthe residue dissolved in ethyl acetate (200 mL)
4. washwashed with water and brine (2×100 mL)
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe resulting residue was purified by flash chromatography (5%MeOH/CH2Cl2)