反应详情

温度

50 °C

To a solution of N-[(1S,2R,3S,4R)-4-(2,6-dichloro-purin-9-yl)-2,3-dihydroxy-cyclopentyl]-propionamide (Intermediate J7) (2.6 g, 7.22 mmol) in dry THF (26 ml) is added C,C-Bis-(4-methoxy-phenyl)-methylamine (Intermediate Y) (3.5 g, 14.44 mmol). The mixture is heated at 50° C. for 12 hours and then concentrated in vacuo. The residue is dissolved in chloroform and washed sequentially with 1.5N HCl, water and saturated aqueous brine solution. The organic phase is dried over anhydrous sodium sulphate and concentrated in vacuo. The crude product is purified by chromatography on silica (60-120 mesh) eluting with 2% methanol in chloroform to afford the title product. LC-MS (0.1% formic acid, acetonitrile): (MH+ 567)

1. concentrationconcentrated in vacuo
2. dissolutionThe residue is dissolved in chloroform
3. washwashed sequentially with 1.5N HCl, water and saturated aqueous brine solution
4. dry with materialThe organic phase is dried over anhydrous sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by chromatography on silica (60-120 mesh)
7. washeluting with 2% methanol in chloroform