反应详情

To a mixture of 2-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]-5-(2H-tetrazol-5-yl)pyrazine from Step 6 (5.00 g, 11.9 mmol) and triethylamine (3.32 mL, 23.8 mmol) in THF (50 mL) at 60° C. was added tert-butyl bromoacetate (3.48 g, 17.9 mmol). After a period of 1 h at 60° C., the reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride. The organic phase was separated, dried over sodium sulfate, filtered and evaporated. To the solid was added 50 mL of acetone followed by slow addition of 100 mL of hexane. The resulting solid was filtered to provide tert-butyl (5-{5-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]pyrazin-2-yl}-2H-tetrazol-2-yl)acetate.

1. customthe reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride
2. customThe organic phase was separated
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customevaporated
6. additionTo the solid was added 50 mL of acetone
7. additionfollowed by slow addition of 100 mL of hexane
8. filtrationThe resulting solid was filtered