HRID846564

反应详情

EQUATION

反应方程式

HRID 846564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a flask were charged 96.2 mg (0.28 mmol) of 4-tetradecanoyloxy benzoic acid, 78.0 mg (0.25 mmol) of 4-hydroxy-4'-(2-methyloctanoyl) biphenyl, 63.5 mg (0.31 mmol) of dicyclohexylcarbodiimide, 3.5 mg (0.03 mmol) of 4-dimethylamino pyridine and 5 ml of dried dichloromethane, which was heated under reflux for 7 hours. After the cooling, the resulting solid was filtered off and washed with dichloromethane. The organic phase was washed with 0.1 normal hydrochloric acid and further with water, dried on anhydrous magnesium sulfate, and the solvent was distilled off. This product was recrystallized with ethanol to obtain 63.5 mg (yield 40%) of white 4-tetradecanoyloxy benzoic acid-4-(2-methyloctanoyl) biphenyl.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hours
  3. filtrationAfter the cooling, the resulting solid was filtered off
  4. washwashed with dichloromethane
  5. washThe organic phase was washed with 0.1 normal hydrochloric acid and further with water
  6. dry with materialdried on anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. customThis product was recrystallized with ethanol