反应详情

温度

110 °C

1-(4-methoxybenzyl)-3-methyl-1H-indazol-5-amine (51 mg, 0.34 mmol) from step 2 of this example, 2-{(1S,2R)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethyl 4-methylbenzenesulfonate from step 1 of Example 5 (75 mg, 0.17 mmol) and potassium iodide (3 mg, 0.017 mmol) combined and the solids slurried in acetonitrile. The slurry was reacted in the microwave with stirring for 80 minutes at 110° C. using normal power. The mixture was cooled to RT, diluted with 4:1 water:saturated sodium bicarbonate (40 ml), extracted with EtOAc (3×40 ml), the organic fractions combined, washed with brine, dried over Na2SO4, filtered and the volatiles removed in vacuum. The product was purified by chromatography on SiO2 eluting with 10% acetone:DCM to give the titled compound.

1. customThe slurry was reacted in the microwave
2. temperatureThe mixture was cooled to RT
3. extractionsaturated sodium bicarbonate (40 ml), extracted with EtOAc (3×40 ml)
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customthe volatiles removed in vacuum
8. customThe product was purified by chromatography on SiO2 eluting with 10% acetone