反应详情

To a solution of 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (3.1 g, 15.5 mmol) and potassium tert-butoxide (1.74 g, 1 eq) in 20 mL THF at 0° C., was added 4,6-dichloropyrimidine (2.3 g, 1 eq). The reaction mixture was stirred for 1 h then a solution of saturated sodium bicarbonate was added. The aqueous layer was extracted with ethyl acetate twice and the combined extracts were washed with a solution of saturated sodium bicarbonate, dried over magnesium sulfate and evaporated. The residue was purified on silica gel (eluent: 20% ethyl acetate in hexane) to give 2.49 g (51% yield) of 3a.

1. extractionThe aqueous layer was extracted with ethyl acetate twice
2. washthe combined extracts were washed with a solution of saturated sodium bicarbonate
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customThe residue was purified on silica gel (eluent: 20% ethyl acetate in hexane)