反应详情

To a solution of 10.0 g. (0.0273 mole) of 1-methyl-4-(10-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine in 50 ml. of dry ether is added 25 ml. of 2-methylfuran and 3.4 g. of potassium t-butoxide. The mixture is stirred and refluxed for 10 days. After the addition of water (1.0 1.), the mixture is extracted with an ether-benzene mixture (4:1). This organic phase is removed, washed with water, dried over magnesium sulfate, filtered, and the solvent is removed on a rotary evaporator. The residue that remains crystallizes readily to give 4.0 g. of product. The material is recrystallized from acetonitrile to give pure 1-methyl-4-(1-methyl-1,4-dihydro-1,4-epoxy-9H-tribenzo[a,c,e]cyclohepten-9-ylidene)piperidine, m.p. 175°-177°.

1. temperaturerefluxed for 10 days
2. extractionthe mixture is extracted with an ether-benzene mixture (4:1)
3. customThis organic phase is removed
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent is removed on a rotary evaporator
8. customThe residue that remains crystallizes readily
9. customto give 4.0 g
10. customThe material is recrystallized from acetonitrile