反应详情

A cooled (0° C.) solution of methyl 2,4-dichloropyrimidine-6-carboxylate (Apollo, OR2558, 10.00 g; 48.31 mmol) in THF (300 mL) was treated with a solution of cyclohexylamine (Fluka, 5.53 mL; 48.3 mmol) and triethylamine (7.37 mL; 53.1 mmol) in THF (100 mL). The reaction mixture was stirred for 16 hours at RT. Water (50 mL) was poured into the reaction mixture which was extracted with EtOAc. The combined organic extracts were dried over magnesium sulfate, filtered and concentrated to obtain the crude product, which was purified by column chromatography (silica) eluting with cyclohexane containing increasing amounts of EtOAc. The title product was obtained as a white solid.

1. extractionwas extracted with EtOAc
2. dry with materialThe combined organic extracts were dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customto obtain the crude product, which
6. customwas purified by column chromatography (silica)
7. washeluting with cyclohexane containing
8. temperatureincreasing amounts of EtOAc