反应详情

2.5 g (13.01 mmol) of N-cyclopropyl-4-(hydroxymethyl)pyridine-2-carboxamide (Example 52A) and 11.76 g (98.84 mmol) of thionyl chloride were combined and stirred at RT overnight. The reaction mixture was concentrated using a rotary evaporator. The residue was dissolved in ethyl acetate and washed once with saturated aqueous sodium bicarbonate solution. The organic phase was dried over magnesium sulfate, filtered and concentrated using a rotary evaporator. The residue was purified by column chromatography on silica gel 60 (mobile phase: cyclohexane/ethyl acetate 2/1).

1. concentrationThe reaction mixture was concentrated
2. customa rotary evaporator
3. dissolutionThe residue was dissolved in ethyl acetate
4. washwashed once with saturated aqueous sodium bicarbonate solution
5. dry with materialThe organic phase was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customa rotary evaporator
9. customThe residue was purified by column chromatography on silica gel 60 (mobile phase: cyclohexane/ethyl acetate 2/1)