HRID616219

反应详情

EQUATION

反应方程式

HRID 616219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.1 g of methylvinylketone are added dropwise at 70° to a solution of 10 g of 4-(10,11-dihydro-5-dibenzo[a,d]cycloheptenylidene)piperidine [M.P. 113°-114°, produced in a manner analogous to that described in Example 4 (a), from 4-(10,11-dihydro-5-dibenzo[a,d]cycloheptenylidene)-1-methylpiperidine] in 100 cc of ethanol, and the mixture is boiled at reflux for 11/2 hours. The reaction mixture is then concentrated by evaporation in a vacuum, the residue is dissolved in acetone, the solution is made acid with hydrogen chloride in ether, is again concentrated by evaporation, and the residue is crystallized first from acetone/ether and then from isopropanol/ether. The hydrochloride of the title compound has an M.P. over 300°.

WORKUP

后处理

  1. customproduced in a manner analogous to
  2. temperatureat reflux for 11/2 hours
  3. concentrationThe reaction mixture is then concentrated by evaporation in a vacuum
  4. dissolutionthe residue is dissolved in acetone
  5. concentrationis again concentrated by evaporation
  6. customthe residue is crystallized first from acetone/ether
  7. customover 300°