反应详情

温度

0 °C

Compound 10e (43 mg, 89.3 mmol) was dissolved in DMF (2 ml) and the solution was cooled to 0° C. and NaH (11 mg, 0.27 mmol) was added. After 0.5 h 2,4-dichloro-pyrimidine was added. The reaction was stirred at 0° C. for 2 h and then quenched by addition of citric acid. The reaction mixture was extracted with DCM (3×10 ml) and the combined organic phases were washed with citric acid, water and brine. The organic phase was dried over MgSO4 and filtered. The solvent was removed in vacuo to yield the crude target compound (43 mg, 81%); LC/MS m/z (ESI+)=595 (MH+).

1. customquenched by addition of citric acid
2. extractionThe reaction mixture was extracted with DCM (3×10 ml)
3. washthe combined organic phases were washed with citric acid, water and brine
4. dry with materialThe organic phase was dried over MgSO4
5. filtrationfiltered
6. customThe solvent was removed in vacuo