反应详情

To a solution of 2,4-dichloro-6-methyl-3-nitropyridine (900 mg, 4.35 mmol) in DMA (8 mL) were added (R)-3-amino-3-phenylpropionic acid ethyl ester HCl (799 mg, 3.48 mmol) and DIPEA (1.6 mL, 8.70 mmol). The reaction mixture was stirred at room temperature for 12 hours. The reaction was then diluted with ethyl acetate and washed with water twice. The organic phase was dried over Na2SO4 and concentrated to give yellow oil. The resulting oily residue was purified by silica gel preparative TLC using 99:1 CH2Cl2:MeOH as an eluent to afford 650 mg (51%) of the title compound as a light orange oil. LCMS, M++1, m/z: 364.15.

1. washwashed with water twice
2. dry with materialThe organic phase was dried over Na2SO4
3. concentrationconcentrated
4. customto give yellow oil
5. customThe resulting oily residue was purified by silica gel preparative TLC