HRID2399735

反应详情

EQUATION

反应方程式

HRID 2399735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Cis-2-triphenylmethylaminocyclohexanol (1.52 g; 4.25 mmol) is added to a solution of sodium hydride (256 mg; 60%; 6.4 mmol) in 20 ml dry THF and refluxed overnight. The solution is cooled, 4-(benzoxazol-2-yl)benzyl bromide (1.3 g; 4.5 mmol) is added in one portion and refluxed for 5 hrs. This is then poured into water and extracted with 2×100 ml CH2Cl2, dried (Na2SO4), concentrated to dryness and flash chromatographed using 4:1 8:1; hexane:EtOAc to obtain Cis-1-[4-(benzoxazol-2-yl)benzyloxy]-2-triphenylmethylaminocyclohexane which is used directly in the next step.

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. temperatureThe solution is cooled
  3. temperaturerefluxed for 5 hrs
  4. extractionextracted with 2×100 ml CH2Cl2
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated to dryness and flash
  7. customchromatographed