反应详情

温度

200 °C

Two 20 mL microwave vials were charged with a half portion of 6-benzyl-4-chloro-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (3.50 g, 13.5 mmol), (R)-1-(4-chloro-phenyl)-ethylamine (4.20 g, 27.0 mmol), N,N-diisopropylethylamine (4.7 mL, 27 mmol) and acetonitrile (20 mL); and the mixture was heated in a microwave at 200° C. for 2.5 h. The mixture was concentrated in vacuo, and the residue was taken up in CH2Cl2 (100 mL) and ethyl acetate (20 mL), washed with 0.5 M aq. NaH2PO4 (pH 4, 100 mL), dried (Na2SO4), and concentrated. The residue was purified on silica gel column (0-5% MeOH/CH2Cl2) to give a pale yellow foam (4.46 g).

1. concentrationThe mixture was concentrated in vacuo
2. washethyl acetate (20 mL), washed with 0.5 M aq. NaH2PO4 (pH 4, 100 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated
5. customThe residue was purified on silica gel column (0-5% MeOH/CH2Cl2)