反应详情

500 mg (1.13 mmol) {1-[4-(2-Bromo-2-phenyl-acetyl)phenyl]-cyclobutyl}-carbamic acid tert.-butyl ester, 137.5 mg (1.13 mmol) 3,5-dimethyl-pyridin-2-yl-amine and molecular sieves (4 Å, dried over night at 120° C. in a drying oven) were heated in 10 mL ethanol in a Dean-Stark apparatus for 23 hours. The reaction mixture had been sucked off via a glass fibre filter and evaporated to dryness. The residue was redissolved in dichloromethane, washed with an 1 M hydrochloric acid, saturated sodium bicarbonate and brine and dried (sodium sulfate). After filtration and removal of the solvent the residue was purified by chromatography on silicagel (eluents: hexane/ethyl acetate) yielding 142.6 mg (25.8%) of the pure title compound and 77.5 mg (14.7%) of the title compound which was slightly contaminated.

1. filtrationfilter
2. customevaporated to dryness
3. dissolutionThe residue was redissolved in dichloromethane
4. washwashed with an 1 M hydrochloric acid, saturated sodium bicarbonate and brine
5. dry with materialdried (sodium sulfate)
6. filtrationAfter filtration and removal of the solvent the residue
7. customwas purified by chromatography on silicagel (eluents: hexane/ethyl acetate)