HRID857589

反应详情

EQUATION

反应方程式

HRID 857589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

44.8 g of 2-methoxy-6-(4-propylcyclohexa-1-ene-1-yl)naphthalene was dissolved in 800 ml of ethyl acetate. To the solution was then added 10 g of 5% palladium carbon. The reaction mixture was then stirred at a hydrogen pressure of 4 kg/cm2 for 6 hours. The catalyst was then removed by filtration. The solvent was then distilled off. The residue was then dissolved in 180 ml of N,N-dimethylformamide. To the solution was then added 18 g of potassium t-butoxide. The reaction mixture was then heated to a temperature of 120° C. with stirring for 1 hour. The reaction solution was then allowed to cool to room temperature. To the reaction solution was then added 70 ml of a 10% hydrochloric acid to causes crystallization. The crystal thus precipitated was filtered off, washed with water, and then dried under reduced pressure. The crystal was then recrystallized from ethanol to obtain 28.0 g of 2-methoxy-6-(trans-4-propylcyclohexyl)naphthalene.

WORKUP

后处理

  1. customThe catalyst was then removed by filtration
  2. distillationThe solvent was then distilled off
  3. dissolutionThe residue was then dissolved in 180 ml of N,N-dimethylformamide
  4. additionTo the solution was then added 18 g of potassium t-butoxide
  5. temperatureto cool to room temperature
  6. additionTo the reaction solution was then added 70 ml of a 10% hydrochloric acid
  7. customto causes crystallization
  8. customThe crystal thus precipitated
  9. filtrationwas filtered off
  10. washwashed with water
  11. customdried under reduced pressure
  12. customThe crystal was then recrystallized from ethanol