HRID612601

反应详情

EQUATION

反应方程式

HRID 612601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepare a stirred mixture of ortho-bromo-phenol (25.951 g, 17.4 mL, 0.15 mole) and potassium carbonate (20.70 g, 0.16 mole) in 175 mL isopropanol at ambient temperature under argon. Slowly add isopropyl iodide (22.2 g, 16.00 mL), heat at reflux and stir the mixture overnight. Cool to ambient temperature then filter, condensing the filtrate on a rotary evaporator. Dissolve the residual oil in diethyl ether (300 mL) and twice extract with 100 mL 50% sodium hyroxide. Separate, wash with brine and concentrate on a rotary evaporator to give a pale yellow liquid. Distill on the Kugelrohr (0.05 mm, 100°-120° C.) to obtain the title compound as an oil. (24.21 g, 75%).

WORKUP

后处理

  1. customPrepare
  2. temperatureat reflux
  3. filtrationthen filter
  4. customcondensing the filtrate
  5. customon a rotary evaporator
  6. dissolutionDissolve the residual oil in diethyl ether (300 mL)
  7. extractiontwice extract with 100 mL 50% sodium hyroxide
  8. customSeparate
  9. washwash with brine
  10. concentrationconcentrate on a rotary evaporator
  11. customto give a pale yellow liquid
  12. distillationDistill on the Kugelrohr (0.05 mm, 100°-120° C.)