反应详情

温度

-40 °C

To a solution of 2-chloro-4-morpholinothieno[3,2-d]pyrimidine 4, Example 2) (1.0 eq) dissolved in THF (0.1M) at −78° C. was added a solution of n-butyllithium (1.3 eq, 1.6M in hexanes) following General Procedure D. The reaction mixture was stirred at −40° C. for 30 minutes. N,N-dimethylacetamide (4.0 eq) was added and reaction mixture was allowed to slowly warm up to 0° C. and stirred for 2 hours. Reaction mixture was poured in a cold solution of 0.25M HCl, and extracted with dichloromethane. The combined organic layers were dried (Na2SO4) and concentrated. The crude reaction mixture was purified by flash chromatography to yield 1-(2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)ethanone.

1. customreaction mixture
2. temperatureto slowly warm up to 0° C.
3. stirringstirred for 2 hours
4. customReaction mixture
5. extractionextracted with dichloromethane
6. dry with materialThe combined organic layers were dried (Na2SO4)
7. concentrationconcentrated
8. customThe crude reaction mixture
9. customwas purified by flash chromatography