反应详情

A suspension of N′-(3-cyano-6-isopropyl-pyridin-2-yl)-N,N-dimethyl-formamidine (2.00 g, 9.3 mmol) and the product from Example 1C (3.46 g, 9.3 mmol) in Acetic acid (40 mL) was heated at 120° C. for 20 minutes under N2. After cooling to room temperature, the reaction mixture was portioned between ethyl acetate (150 mL) and H2 (200 mL), and then made basic to pH 9 with K2CO3 under stirring. The organic layer was separated, washed with 10% NaHCO3, H2O and brine, dried over MgSO4, and evaporated to give a pale brown oil. The oily residue was separated by silica gel column chromatography (ethyl acetate/n-hexane=5/1) gave yellow crystal. Further purification by washing with cold ethyl acetate (15 mL) gave the title compound as slightly yellow crystal (3.27 g, 65% yield).

1. customThe organic layer was separated
2. washwashed with 10% NaHCO3, H2O and brine
3. dry with materialdried over MgSO4
4. customevaporated
5. customto give a pale brown oil
6. customThe oily residue was separated by silica gel column chromatography (ethyl acetate/n-hexane=5/1)
7. customgave yellow crystal
8. customFurther purification
9. washby washing with cold ethyl acetate (15 mL)