HRID1902676

反应详情

EQUATION

反应方程式

HRID 1902676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7.37 g. (0.030 moles) of 3-[N,N-diphenylamino]-1-chloropropane, 6.0 g. (0.024 moles) of 4-(3-methylphenyl)-piperidine hydrochloride, 3.92 g. (0.024 moles) of potassium iodide, and 5.30 g. (0.050 moles) of sodium carbonate in 60 ml. of n-butanol is refluxed for about 16 hours. Solvent is evaporated and the residue is dissolved in chloroform and washed with water. The chloroform solution is dried and passed through a column of silica gel. The product is eluted with acetonitrile. The product fractions are combined, concentrated, and converted to the maleate salt in ether. The resulting crystals recrystallized from acetonitrile to give 7.2 g. of N,N-diphenyl-4-[3-methylphenyl]-1-piperidinepropanamine butanedioate (1:1), mp. 137.5°-139.5° C.

WORKUP

后处理

  1. additionA mixture of 7.37 g
  2. customSolvent is evaporated
  3. dissolutionthe residue is dissolved in chloroform
  4. washwashed with water
  5. dry with materialThe chloroform solution is dried
  6. washThe product is eluted with acetonitrile
  7. concentrationconcentrated
  8. customThe resulting crystals recrystallized from acetonitrile
  9. customto give 7.2 g