反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureat reflux temperature for about 24 hours
- temperatureto cool
- customevaporated
- customThe residue from the evaporation
- customThe resultant layers were separated
- washthe aqueous layer was washed with chloroform
- dry with materialThe organic layer was dried over sodium sulfate overnight
- washafter which it was again washed with a volume of chloroform
- customevaporated
- temperatureheated on a steam bath