HRID2950

反应详情

EQUATION

反应方程式

HRID 2950 的结构方程式

PROCEDURE

实验过程

Under a nitrogen atmosphere, 76.65 g of 2-(1,1-dimethylethyl)-6-methylphenol (Aldrich), 65.42 g of hexamethylenetetramine and 700 ml of trifluoroacetic acid were stirred at reflux temperature for about 24 hours, then allowed to cool and evaporated. The residue from the evaporation was taken up in 1500 ml of water and 1000 ml of chloroform and neutralized to pH 7 with solid sodium carbonate. The resultant layers were separated and the aqueous layer was washed with chloroform. The organic layer was dried over sodium sulfate overnight, after which it was again washed with a volume of chloroform and evaporated. The resultant residue was then taken up in 375 ml of toluene, heated on a steam bath and then allowed to cool to room temperature overnight. Subsequent workup gave 28.3 g of the desired subtitled intermediate.

WORKUP

后处理

  1. temperatureat reflux temperature for about 24 hours
  2. temperatureto cool
  3. customevaporated
  4. customThe residue from the evaporation
  5. customThe resultant layers were separated
  6. washthe aqueous layer was washed with chloroform
  7. dry with materialThe organic layer was dried over sodium sulfate overnight
  8. washafter which it was again washed with a volume of chloroform
  9. customevaporated
  10. temperatureheated on a steam bath