反应详情

A stirred solution of 4-methylbenzyl 4-(aminomethyl)-1-piperidinecarboxylate (INTERMEDIATE 2A) (20.00 g, 76.23 mmol), 2-chloro-pyrimidine (8.73 g, 76.23 mmol) and triethylamine (21.25 mL, 152.46 mmol) in DMF (40 mL) was heated at 100° C. for 6 h. The reaction solution was cooled to rt, then diluted with ethyl acetate (800 mL), washed with sat. aq. NaHCO3 (100 mL), water (3×100 mL), brine (100 mL), dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel chromatography (CH2Cl2/IPA/hexanes) to give 4-methylbenzyl 4-[(2-pyrimidinylamino)methyl]-1-piperidinecarboxylate. M.S. (M+1): 341.30

1. washwashed with sat. aq. NaHCO3 (100 mL), water (3×100 mL), brine (100 mL)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography (CH2Cl2/IPA/hexanes)