反应详情

温度

75 °C

To a solution of ethyl ({4-amino-6-chloro-2-[(E)-2-phenylethenyl]-5-pyrimidinyl}oxy)acetate (0.55 g, 1.65 mmol) in DMF (5 mL) was added solid K2CO3 (0.46 g, 3.3 mmol) and the resulting mixture was heated at 75° C. for 1 h. The solvent was evaporated under reduced pressure and the residue was extracted with 10% methanol in DCM (3×100 ml). The organic extracts were combined, dried over anhydrous MgSO4, filtered and evaporated under reduced pressure to give a solid which was purified by column chromatography (silica gel) with a 0-10% methanol in DCM gradient to give the desired product as a solid (0.47 g, 99%).

1. customThe solvent was evaporated under reduced pressure
2. extractionthe residue was extracted with 10% methanol in DCM (3×100 ml)
3. dry with materialdried over anhydrous MgSO4
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customto give a solid which
7. customwas purified by column chromatography (silica gel) with a 0-10% methanol in DCM gradient