反应详情

Combine 1.00 g (4.76 mmole) 1-chloro-2-(4-chloro-2- butenyl)benzene and 1.77 g (4.76 mmole) N,N-diethylheptanamine and heat at 100° C. ca. 20 hrs. Follow the progress of the reaction by TLC on silica gel (acetonitrile: ammonium hydroxide, 9:1). At the completion of the reaction, decant off the top layer of the two phase reaction mixture. Dissolve the bottom layer in 50 ml H2O. Extract with 3×100 ml hexane, 1×25 ml CH2Cl2. Dry CH2Cl2 over MgSO4 and treat with activated charcoal. Evaporate the solvents to provide the title compound.

1. customthe progress of the reaction by TLC on silica gel (acetonitrile: ammonium hydroxide, 9:1)
2. customAt the completion of the reaction
3. customdecant off
4. customthe top layer of the two phase reaction mixture
5. extractionExtract with 3×100 ml hexane, 1×25 ml CH2Cl2
6. additionDry CH2Cl2 over MgSO4 and treat with activated charcoal
7. customEvaporate the solvents