反应详情

温度

110 °C

In a schlenck tube, a mixture of 2-(2-(2-chlorophenyl)pyrimidin-5-ylamino)-5-cyclopropylbenzoic acid (0.55 mmol, 0.200 g), cyclopropylboronic acid (0.71 mmol, 0.061 g), K3PO4 (1.86 mmol, 0.395 g), PCy3 (0.05 mmol, 0.015 g) and Pd(AcO)2 (0.03 mmol, 0.006 g) in a mixture of toluene/water 6:1 (6 ml) was heated at 110° C. for 72 hours, under argon atmosphere. The crude mixture was poured into water and extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered and the solvent removed. The crude mixture was purified by reverse phase chromatography eluting with a gradient of 100% water to 100% MeOH/AcN 1:1 affording 0.016 g (71% of yield).

1. extractionextracted with ethyl acetate
2. dry with materialThe organic phase was dried over MgSO4
3. filtrationfiltered
4. customthe solvent removed
5. customThe crude mixture was purified by reverse phase chromatography
6. washeluting with a gradient of 100% water to 100% MeOH/AcN 1:1 affording 0.016 g (71% of yield)