反应详情

温度

140 °C

A mixture of 1-(5-bromopyrimidin-2-yl)piperidin-4-ol (5 g, 19.37 mmol) and copper(I) cyanide (6.94 g, 77 mmol) in DMF (48.4 mL) was heated at 140° C. for 18 h. The mixture was diluted with water (100 mL) and EtOAc (50 mL) and filtered through celite. The filtrate was extracted with EtOAc (3×20 mL). The combined organic fractions were washed with 1N HCl (20 mL) then dried over Na2SO4. The solvent was evaporated and the product was recrystallized from CH2Cl2/hexanes, filtered and washed with hexanes to afford the title compound.

1. filtrationfiltered through celite
2. extractionThe filtrate was extracted with EtOAc (3×20 mL)
3. washThe combined organic fractions were washed with 1N HCl (20 mL)
4. dry with materialthen dried over Na2SO4
5. customThe solvent was evaporated
6. customthe product was recrystallized from CH2Cl2/hexanes
7. filtrationfiltered
8. washwashed with hexanes