反应详情

To 6-chloro-9H-purin-2-ylamine (20 g, 0.12 moles) in DMF (200 mL) at −11° C. was added NaH (5.7 g, 0.14 moles, 60%) portionwise over 1 h. The mixture as stirred for 1 h, then 2-iodopropane (14.2 mL, 0.14 moles) was added dropwise. The solution was warmed to rt, stirred for 18 h, quenched with sat'd NH4Cl, and extracted with EtOAc. The combined extracts, were washed with water, sat'd NaCl, then dried over MgSO4 and filtered. Concentration yielded an oil which was purified by silica gel chromatography (60% EtOAc/Hexane) to a white solid (13.4 g, 54%): MS [M+H]+ 212; m.p. 135–136° C.

1. stirringstirred for 18 h
2. customquenched with sat'd NH4Cl
3. extractionextracted with EtOAc
4. washThe combined extracts, were washed with water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationConcentration
8. customyielded an oil which
9. customwas purified by silica gel chromatography (60% EtOAc/Hexane) to a white solid (13.4 g, 54%)