HRID45837

反应详情

EQUATION

反应方程式

HRID 45837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 mg (0.4 mmol) of N-(diphenylmethylidene)-3-[1-(4-methoxybenzyl)-4-(1-oxidopyridin-4-yl)-1H-pyrazol-3-yl]aniline were suspended in 50 ml of trifluoromethylbenzene and 210 μl (2 mmol) of tert-butylamine were added under stirring at room temperature. The mixture was cooled to 0° C. and 260 mg (0.8 mmol) of p-toluensulfonic anhydride were added. The reaction was maintained in the same conditions for 2.5 hours. Then the same amounts of reactants and 2 ml of dichloromethane to obtain a clear solution were added and after further 2 hours the reaction went to completion. The solvent was evaporated and the residue taken up in dichloromethane and washed with water. The organic phase was dried over Na2SO4 and evaporated to dryness, giving 161 mg (73% yield) of the title compound.

WORKUP

后处理

  1. temperatureThe mixture was cooled to 0° C.
  2. temperatureThe reaction was maintained in the same conditions for 2.5 hours
  3. additionwere added and after further 2 hours the reaction
  4. customThe solvent was evaporated
  5. washwashed with water
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customevaporated to dryness