反应详情

温度

20 °C

In a nitrogen purged sealed tube was dissolved N-(4-(7-methoxy-1,5-naphthyridin-4-yloxy)phenyl)-4-(4-(2-(triethylsilyl)ethynyl)phenyl)phthalazin-1-amine (0.100 g, 0.164 mmol) in MeOH (2.00 mL). Potassium carbonate (0.068 g, 0.492 mmol) was added and the reaction was stirred at 20° C. for 24 h and then concentrated. The crude was extracted into DCM, washed 1× with water, 1× with brine, dried over Na2SO4, filtered through flitted funnel, concentrated. The resulting crude material was purified by silica gel chromatography eluting with 0-100% CH2Cl2:MeOH(90:10)/CH2Cl2. The product fractions were concentrated to afford 4-(4-ethynylphenyl)-N-(4-(7-methoxy-1,5-naphthyridin-4-yloxy)phenyl)phthalazin-1-amine as light yellow solid. MS [M+H]=496; Calc'd 495.5 for C31H21N5O2.

1. customIn a nitrogen purged
2. customsealed tube
3. concentrationconcentrated
4. extractionThe crude was extracted into DCM
5. washwashed 1× with water, 1× with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered through flitted funnel
8. concentrationconcentrated
9. customThe resulting crude material was purified by silica gel chromatography
10. washeluting with 0-100% CH2Cl2:MeOH(90:10)/CH2Cl2
11. concentrationThe product fractions were concentrated