反应详情

温度

110 °C

A stirred mixture of ethyl 1-(5-(7-bromo-2-(3-ethylureido)benzo[d]thiazol-5-yl)pyrimidin-2-yl)-4-methylpiperidine-4-carboxylate (150 mg, 0.274 mmol), tetrakis(triphenylphosphine)palladium (16 mg, 0.0138 mmol) and 2-methoxy-4-(tributylstannyl)thiazole (0.33 mL, 0.822 mmol) in anhydrous DMF (3.0 mL) was purged with N2 for 20 min. The reaction vessel was sealed and heated at 110° C. for 10 h. After cooling to rt, the mixture was diluted with water (50 mL) and extracted with EtOAc (3×20 mL) which was washed with brine (30 mL) and dried (MgSO4). The solvent was removed in vacuo and the residue purified by flash silica chromatography eluting with 0 to 100% EtOAc in iso-hexane to give 99 mg of the desired product as an off white gummy solid.

1. customwas purged with N2 for 20 min
2. customThe reaction vessel was sealed
3. temperatureAfter cooling to rt
4. additionthe mixture was diluted with water (50 mL)
5. extractionextracted with EtOAc (3×20 mL) which
6. washwas washed with brine (30 mL)
7. dry with materialdried (MgSO4)
8. customThe solvent was removed in vacuo
9. customthe residue purified by flash silica chromatography
10. washeluting with 0 to 100% EtOAc in iso-hexane