HRID36611

反应详情

EQUATION

反应方程式

HRID 36611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a solution of partially dissolved piperazine (15.2 g, 0.17 mmol) in THF (130 mL) at more temperature was added dropwise a solution of 5-chloro-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2.3g, 10.3 mmol) in 20 mL THF. The reaction was allowed to stir overnight and then was diluted with CH2Cl2, washed once with 1.0N NaOH solution, once with brine and then dried (Mg SO4). It was then filtered and the solvent removed to give a residue which was flash chromatographed (5% MeOH saturated with NH3 in CH2Cl2) to give 1.38 g of a glassy solid of the title compound.

WORKUP

后处理

  1. washwashed once with 1.0N NaOH solution, once with brine
  2. dry with materialdried (Mg SO4)
  3. filtrationIt was then filtered
  4. customthe solvent removed
  5. customto give a residue which
  6. customchromatographed (5% MeOH saturated with NH3 in CH2Cl2)