反应详情

温度

100 °C

In a dried pressure flask was placed compound 2 (1.0 g, 3.70 mmol), 4-aminopyrimidine (352 mg, 3.7 mmol), sodium phenoxide (860 mg, 7.4 mmol), Pd2(dba)3 (170 mg, 5 mol %), and Xantphos (150 mg, 7 mol %). The flask was evacuated and filled with N2 3× and then 20 mL anhydrous dioxane was added, The mixture was heated at 100° C. for 12 hours. The cooled mixture was diluted with ethyl acetate and water, filtered, separated, the ethyl acetate layer extracted 1× with ethyl acetate, the combined ethyl acetate layers washed with brine 4×, dried over Na2SO4, filtered and concentrated. The product was purified by column chromatography (silica) CH2Cl2/MeOH to give 3.

1. customIn a dried pressure flask was placed
2. customThe flask was evacuated
3. additionfilled with N2 3×
4. addition20 mL anhydrous dioxane was added
5. additionThe cooled mixture was diluted with ethyl acetate and water
6. filtrationfiltered
7. customseparated
8. extractionthe ethyl acetate layer extracted 1× with ethyl acetate
9. washthe combined ethyl acetate layers washed with brine 4×
10. dry with materialdried over Na2SO4
11. filtrationfiltered
12. concentrationconcentrated
13. customThe product was purified by column chromatography (silica) CH2Cl2/MeOH
14. customto give 3