反应详情

1-Methyl-4-(10-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine, 7.32 g. (0.02mole) is dissolved in 100 ml. of dry piperidine. To this solution is added slowly 25 ml. of a 1.6M solution of butyl lithium in hexane (0.04 mole) under anhydrous conditions and then stirred and refluxed for 8 hours under anhydrous conditions. The reaction is cooled and poured into 500 ml. of benzene and extracted 6 times with 100 ml. of water. The benzene is dried over anhydrous MgSO4, filtered, and the benzene removed on a rotary evaporator leaving 1-methyl-4-(10-(1-piperidyl)-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine as an oil which still has some solvent in it.

1. dissolution(0.02mole) is dissolved in 100 ml
2. additionTo this solution is added slowly 25 ml
3. temperaturerefluxed for 8 hours under anhydrous conditions
4. temperatureThe reaction is cooled
5. additionpoured into 500 ml
6. extractionof benzene and extracted 6 times with 100 ml
7. dry with materialThe benzene is dried over anhydrous MgSO4
8. filtrationfiltered
9. customthe benzene removed on a rotary evaporator