HRID917843

反应详情

EQUATION

反应方程式

HRID 917843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Methyl-4-(10-(1-piperidyl)-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine, 2.4 g., is refluxed for 4 hours with 100 ml. of 10% HCl in water and 50 ml. of methanol. The methanol is evaporated and the remaining oil and water is made basic with solid NaHCO3 until no more CO2 is evolved. It is then extracted three times with 50 ml. each of toluene, combined extracts dried over MgSO4, filtered, and the toluene evaporated on a rotary evaporator leaving a residual product which crystallizes on standing. Three recrystallizations of this product from hexane gives 1-methyl-4-(10,11-dihydro-10-oxo-dibenzo[a,d]cyclohepten-5-ylidene)piperidine, m.p. 142°-143°C.

WORKUP

后处理

  1. temperature, is refluxed for 4 hours with 100 ml
  2. customThe methanol is evaporated
  3. extractionIt is then extracted three times with 50 ml
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe toluene evaporated on a rotary evaporator
  7. customleaving a residual product which
  8. customcrystallizes on standing
  9. customThree recrystallizations of this product from hexane