反应详情

温度

20 °C

In 4 separate microwave vessels were added equal amounts of the following (total/4): dissolved 4-aminophenol (0.054 g, 0.498 mmol) in 1-methyl-2-pyrrolidinone (4.7 mL), added cesium carbonate (0.309 g, 0.948 mmol). Each mixture was stirred at 20° C. for 5 minutes, after which was added 2-chloro-3-(1-trityl-1H-pyrazol-4-yl)pyridine (0.200 g, 0.474 mmol) and heated to 200° C. in the microwave for 6 minutes. The solutions were combined and extracted into EtOAc, washed 1×H2O, 1×NaCl, dried with Mg2SO4, filtered through fritted funnel, and concentrated. The crude residue was purified by silica gel chromatography using 25-70% EtOAc/Hexanes. The product fraction were concentrated to yield 4-(3-(1-trityl-1H-pyrazol-4-yl)pyridin-2-yloxy)benzenamine as brown oil. MS m/z=495 [M+1]+. Calc'd for C33H26N4O: 494.59.

1. customIn 4 separate microwave vessels
2. additionwere added equal amounts of the following (total/4)
3. temperatureheated to 200° C. in the microwave for 6 minutes
4. extractionextracted into EtOAc
5. washwashed 1×H2O, 1×NaCl
6. dry with materialdried with Mg2SO4
7. filtrationfiltered through fritted funnel
8. concentrationconcentrated
9. customThe crude residue was purified by silica gel chromatography
10. concentrationThe product fraction were concentrated