反应详情

温度

130 °C

1.25 g (2.81 mmol) {1-[4-(2-Bromo-2-phenyl-acetyl)phenyl]-cyclobutyl}-carbamic acid tert.-butyl ester, 631.4 mg (3.38 mmol) 2-amino-5-bromo-3-methyl-pyridine, 2.15 g molecular sieves (4 Å, dried over night at 120° C. in a drying oven), 363.5 mg (2.81 mmol) N,N-diisopropylethylamine in 12 mL 2-propanol (degassed for 15′) in a microwave vial, sealed with a microwave cap, were heated at 130° C. for 17 hours in a heating block. The reaction mixture was sucked off via a glass fibre filter and the filter was washed with dichloromethane. After evaporation to dryness, the residue was redissolved in dichloromethane (200 mL), washed with an 1 M hydrochloric acid (50 mL), saturated sodium bicarbonate (50 mL) and brine (100 mL) and dried (sodium sulfate). After filtration and removal of the solvent the residue was purified by chromatography on silicagel (eluents: hexane/ethyl acetate) yielding 256.7 mg (17.1%) of the title compound.

1. customdegassed for 15′) in a microwave vial
2. customsealed with a microwave
3. customcap
4. filtrationfilter
5. washthe filter was washed with dichloromethane
6. customAfter evaporation to dryness
7. dissolutionthe residue was redissolved in dichloromethane (200 mL)
8. washwashed with an 1 M hydrochloric acid (50 mL), saturated sodium bicarbonate (50 mL) and brine (100 mL)
9. dry with materialdried (sodium sulfate)
10. filtrationAfter filtration and removal of the solvent the residue
11. customwas purified by chromatography on silicagel (eluents: hexane/ethyl acetate)