反应详情

n-Butyllithium (2.5M, 1.45 ml) was added to a stirred cooled solution of 1-bromo-2-[2-(methylsulphenyl)-4-trifluoromethylphenyl]acetylene and 1,1-dibromo-2-[2-(methylsulphenyl)-4-trifluoromethylphenyl]ethene (1.0 g) in THF, maintaining the temperature below -70° C. The mixture was stirred for 30 minutes and cyclopropanecarbonyl chloride (0.75 g) was added. The temperature was allowed to rise to room temperature and the mixture was stirred for 2 hours, aqueous ammonium chloride was added and the mixture was extracted with ether, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was purified by chromotography eluted with a mixture of hexane and ether to give 3-cyclopropyl-1-[2-(methylsulphenyl)-4-trifluoromethylphenyl]prop-1-yn-3-one (0.64 g) as yellow oil, NMR (CDCI3) 1.15(m,2H), 1.45(m,2H), 2.2(m,1H), 2.6(s,1H), 7.35(d,1H) 7.4(s,1H), 7.6(d,1H).

1. temperaturemaintaining the temperature below -70° C
2. customto rise to room temperature
3. stirringthe mixture was stirred for 2 hours
4. extractionthe mixture was extracted with ether
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customThe flitrate was evaporated to dryness
8. customthe residue was purified by chromotography
9. washeluted with a mixture of hexane and ether