反应详情

To a mixture of 4-(2-oxo-ethyl)-piperidine-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester (324 mg, 1.08 mmol) and 5-amino-2-chloropyrimidine (140 mg, 1.08 mmol) in DCE (3 mL) was added AcOH (0.19 mL, 3.4 mmol) followed by NaBH(OAc)3 (687 mg, 3.24 mmol) and then stirred for 18 hours at ambient temperature. Water was added and the solution was brought to pH 9 with NH4OH. The two layers were separated and the aqueous was extracted with CH2Cl2, dried over Na2SO4, filtered and concentrated to afford a solid which was purified by flash column chromatography (5 to 50% EtOAc/Heptane) to provide 188 mg (42% yield) of the title compound.

1. customThe two layers were separated
2. extractionthe aqueous was extracted with CH2Cl2
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto afford a solid which
7. customwas purified by flash column chromatography (5 to 50% EtOAc/Heptane)