HRID418702

反应详情

EQUATION

反应方程式

HRID 418702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of aniline (2 mL, 21.9 mmol), trifluoroacetaldehyde ethyl hemiacetal (2.6 mL, 21.9 mmol) and p-toluenesulfonic acid monohydrate (220 mg, 1.16 mmol) in ethanol (25 mL) was heated to reflux for 3 h under continuous stirring. The reaction mixture was cooled, the solvent was removed under reduced pressure and the residue was dissolved in EtOAc. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate, dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to afford title compound 325 (4.16 g, crude) as a yellow oil which was used directly for the next step.

WORKUP

后处理

  1. temperatureto reflux for 3 h under continuous stirring
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in EtOAc
  5. washThe organic layer was washed with a saturated aqueous solution of sodium bicarbonate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was removed under reduced pressure