反应详情

A solution of ethyl 3-(chloromethyl)-2-methyl-2-(3-nitrophenyl)cyclopropane carboxylate (Preparation 5, 1 g, 3.36 rmnol) in 3-cyclohexylpropylamine ([Preparation—Eur. J. Med. Chem. (1992), 27, 321-330], 2.9 g, 20.5 mmol) was heated to 160° C. for 16 h. The mixture was cooled, 2N hydrochloric acid solution (20 ml) was added and the mixture was extracted with dichloromethane (3×20 ml). The combined extracts were dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by silica (200 g) column chromatography eluting with dichloromethane then diethyl ether. Appropriate fractions were combined and concentrated in vacuo to give the title compound as an amber oil (870 mg, 73%).

1. temperatureThe mixture was cooled
2. extractionthe mixture was extracted with dichloromethane (3×20 ml)
3. dry with materialThe combined extracts were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica (200 g) column chromatography
7. washeluting with dichloromethane
8. concentrationconcentrated in vacuo