HRID326968

反应详情

EQUATION

反应方程式

HRID 326968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Using a 30-ml flask similar to that used in Production Example 1, 0.65 g (2.84 mmole) of 4.4'-dimethoxydiphenylamine and 5 mg of p-toluenesulfonic acid monohydrate were added to 10 ml anhydrous toluene solution containing 1.11 g (2.84 mmole) of 1,1-bis(p-2,2,2-trifluoroethoxyphenylacetaldehyde under a nitrogen atmosphere, and refluxed for 3 hours while dehydrating using molecular sieves 4A. After cooling to room temperature, the solution was filtered and the solvent was distilled off. The residue was purified using an alumina column (toluene). The resulting white solid was recrystallized from hexane to yield white crystals of 1,1-bis(p-2,2,2-trifluoroethoxyphenyl)-2-[N,N-bis-(4-methoxyphenyl)amino]ethylene [Compound (4)] in an amount of 1.46 g (yield 85%).

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. filtrationthe solution was filtered
  3. distillationthe solvent was distilled off
  4. customThe residue was purified
  5. customThe resulting white solid was recrystallized from hexane