HRID612601
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customPrepare
- temperatureat reflux
- filtrationthen filter
- customcondensing the filtrate
- customon a rotary evaporator
- dissolutionDissolve the residual oil in diethyl ether (300 mL)
- extractiontwice extract with 100 mL 50% sodium hyroxide
- customSeparate
- washwash with brine
- concentrationconcentrate on a rotary evaporator
- customto give a pale yellow liquid
- distillationDistill on the Kugelrohr (0.05 mm, 100°-120° C.)