反应详情

A solution of 3.3 g of (E)-4-(4-isoquinolinyl)-3-buten-1-ol in 15 mL of dry chloroform was added to a cold solution of 1.8 mL of thionyl chloride in 5 mL of dry chloroform. After 15 minutes, the cooling bath was removed and the reaction was stirred at room temperature for 1 hour and then at reflux for 3 hours. The cooled mixture was washed with NaHCO3 solution and with brine, then was dried (Na2SO4) and evaporated. The residue was purified by chromatography over silica gel (ethyl acetate-toluene; 3:17) to yield 2.2 g of (E)-4-(4-chloro-1-butenyl)isoquinoline as an oil.

1. customthe cooling bath was removed
2. temperatureat reflux for 3 hours
3. washThe cooled mixture was washed with NaHCO3 solution and with brine
4. dry with materialwas dried (Na2SO4)
5. customevaporated
6. customThe residue was purified by chromatography over silica gel (ethyl acetate-toluene; 3:17)