反应详情

Cs2CO3 (382 g, 1.2 mol) was added to a solution of 4-Chloro-7H-pyrrolo[2,3-d]pyrimidine (120 g, 0.78 mol) in DMF (1.0 L) at room temperature. The resulting mixture was stirred for 30 min. 2-Iodopropane (267 g, 1.6 mol) was added and the reaction and stirred for 5 h at room temperature. The reaction mixture was filtered and the solid was washed with EtOAc (3×500 mL). The combined filtrates were washed with water (3×500 mL) and brine (3×250 mL), dried (Na2SO4), filtered, and concentrated in vacuo to afford the title compound as a yellow solid (151 g, 94%). MS: 19.6 (MH+); HPLC Rf: 4.89 min. (HPLC method 4).

1. customthe reaction
2. stirringstirred for 5 h at room temperature
3. filtrationThe reaction mixture was filtered
4. washthe solid was washed with EtOAc (3×500 mL)
5. washThe combined filtrates were washed with water (3×500 mL) and brine (3×250 mL)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo