HRID864493

反应详情

EQUATION

反应方程式

HRID 864493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a cooled (-80° C.) solution of ((3,5-bis(trifluoromethyl)phenyl)methyloxy)acetonitrile (0.51 g; Example 1a, Method B(i) was added 0.42M lithio diphenylmethane (10 ml; prepared by addition of 2.5M n-butyl lithium in hexane (10 ml) to a cooled (-80° C.) solution of diphenylmethane (4.2 g) in diethyl ether (5 ml), followed by warming to room temperature for 3 hours). The solution was warmed to room temperature for 0.5h and then 1M-hydrochloric acid (10 ml) and ethyl acetate were added and the organic phase washed with saturated brine and dried (MgSO4). After evaporation in vacuo the residue was chromatographed on silica gel (eluting with 5% ethyl acetate in hexane ) to give 1-(3,5-bis(triflouromethyl)phenyl)methyloxy)-3,3-diphenyl acetone as an oil which gave an identical 1H NMR spectrum to the material prepared by Method A.

WORKUP

后处理

  1. washthe organic phase washed with saturated brine
  2. dry with materialdried (MgSO4)
  3. customAfter evaporation in vacuo the residue
  4. customwas chromatographed on silica gel (eluting with 5% ethyl acetate in hexane )