反应详情

1-Methyl-4-(10-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine, 2.87 g. (0.0079 mole), 50 ml. of a 0.4M solution of potassium t-butoxide in t-butanol, and 20 ml. of dry piperidine is stirred and refluxed under anhydrous conditions for 6 hours. The reaction mixture is cooled and partitioned between 350 ml. of benzene and 50 ml. of water. The benzene layer is then extracted 5 more times with 50 ml. each of water. The benzene layer is then dried over anhydrous MgSO4, filtered, and the benzene evaporated. This gives a single spot on t.l.c. and is used directly in the next step.

1. temperaturerefluxed under anhydrous conditions for 6 hours
2. temperatureThe reaction mixture is cooled
3. custompartitioned between 350 ml
4. extractionThe benzene layer is then extracted 5 more times with 50 ml
5. dry with materialThe benzene layer is then dried over anhydrous MgSO4
6. filtrationfiltered
7. customthe benzene evaporated
8. customThis gives a single spot on t.l.c