反应详情

温度

-78 °C

To 4-methyl-3-[3-(2-methylamino-pyrimidin-4-yl)-pyridin-2-yloxy]-benzoyl chloride (50 mg, 0.14 mmol) in a flame dried, round-bottom flask under nitrogen and cooled to −78° C. was added 4 ml of THF, 2 ml methylene chloride and magnesium-bromide-2-methoxy-benzene in THF (0.3 ml, 0.6 mmol). After addition of the magnesium-bromide, the −78° C. dry ice bath was removed and the reaction allowed to warm to room temperature over 4 h. The reaction was quenched with saturated sodium bicarbonate solution and extracted with methylene chloride and brine. The organic layers were combined, dried with sodium sulfate and filtered. The solvent was removed under vacuum and the product was purified via preparative HPLC (Gilson). MS m/z=427 [M+H]+. Calc'd for C25H22N4O3: 426.48.

1. customthe −78° C. dry ice bath was removed
2. temperatureto warm to room temperature over 4 h
3. customThe reaction was quenched with saturated sodium bicarbonate solution
4. extractionextracted with methylene chloride and brine
5. dry with materialdried with sodium sulfate
6. filtrationfiltered
7. customThe solvent was removed under vacuum
8. customthe product was purified via preparative HPLC (Gilson)