反应详情

A solution of 2-amino-5-cyano pyridine (2.0 g) in dry dichloromethane (17 mL) under nitrogen at 0° C. was treated with triethylamine (2.6 mL) followed by slow addition of chloroacetyl chloride (1.5 mL). The reaction mixture was allowed to warm up to room temperature. After 2 h, the mixture was partitioned between dichloromethane and water. The phases were separated and the aqueous layer was extracted with dichloromethane (×2). The combined organic layer was washed with brine, dried over sodium sulphate, filtered and concentrated to give the crude product which was purified by silica gel chromatography eluting with 50% EtOAc/cyclohexane. The relevant fractions were combined and evaporated to give the title compound (2.17 g) as a light brown solid.

1. customthe mixture was partitioned between dichloromethane and water
2. customThe phases were separated
3. extractionthe aqueous layer was extracted with dichloromethane (×2)
4. washThe combined organic layer was washed with brine
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated
8. customto give the crude product which
9. customwas purified by silica gel chromatography
10. washeluting with 50% EtOAc/cyclohexane
11. customevaporated