HRID2269227

反应详情

EQUATION

反应方程式

HRID 2269227 的结构方程式

PROCEDURE

实验过程

Trifluoroacetic acid (35 ml), was mixed with 3.93 g(20.0 mmol), of 2,2-diphenylpropane and 2.80 g (20.0 mmol), of hexamethylenetetramine and heated to reflux for 16 hours. After cooling to room temperature, the reaction mixture was poured into ice water and the mixture was stirred for 1 hour. The solution was adjusted to pH=about 9 and extracted with 100 ml of diethyl ether. The organic extract was washed with saturated saline and dried with sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1), to obtain 3.61 g (yield: 80.5%), of the target compound as a pale yellow oily substance.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 16 hours
  3. extractionextracted with 100 ml of diethyl ether
  4. extractionThe organic extract
  5. washwas washed with saturated saline
  6. dry with materialdried with sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)
  9. customto obtain 3.61 g (yield: 80.5%)