反应详情

To a solution of 2.00 g. (0.00545 mole) of 1-methyl-4-(1-methyl-1,4-dihydro-1,4-epoxy-9H-tribenzo[a,c,e]cyclohepten-9-ylidene)piperidine and 2.16 g. (0.0056 mole) of tetraphenylcyclopentadienone in 60 ml. of xylene (b.p. 139°-140°) is stirred and refluxed for 20 hours. After cooling, 30 ml. of 6N hydrochloric acid is added. The precipitate that forms is removed by filtration and the solid precipitate is washed with ether and benzene. The solid is collected and made basic with 40% sodium hydroxide solution. The mixture is extracted with ether, and the ether extract is washed with water and dried over magnesium sulfate. After filtration, the ether is removed to give a crystalline residue which is recrystallized from methanol to give 1-methyl-4-(1-methyl-8H-dibenzo[a,e]furo[3,4-c]cyclohepten-8-ylidene)piperidine, m.p. 80°-86°.

1. temperaturerefluxed for 20 hours
2. temperatureAfter cooling
3. customThe precipitate that forms is removed by filtration
4. washthe solid precipitate is washed with ether and benzene
5. customThe solid is collected
6. extractionThe mixture is extracted with ether
7. extractionthe ether extract
8. washis washed with water
9. dry with materialdried over magnesium sulfate
10. filtrationAfter filtration
11. customthe ether is removed
12. customto give a crystalline residue which
13. customis recrystallized from methanol