HRID1156644

反应详情

EQUATION

反应方程式

HRID 1156644 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 45.0 g of 4-(2-bromoethoxy)-phenol (0.207 mol) in 310 ml of acetone was added 54 ml of allyl bromide (0.619 mol) and 45.0 g of anhydrous potassium carbonate (0.326 mol). The reaction mixture was stirred under reflux for eleven hours and was cooled and poured into 2500 ml of water. The mixture was extracted twice with 3:1 ether:methylene-chloride, and the organic layers were washed twice with 1 N NaOH, once with H2O, dried (Na2SO4) and concentrated to dryness under reduced pressure to yield a colorless oil. The analytical sample was prepared by crystallization from hexane to give colorless crystals, mp 27°-28°.

WORKUP

后处理

  1. temperatureunder reflux for eleven hours
  2. temperaturewas cooled
  3. extractionThe mixture was extracted twice with 3:1 ether
  4. washmethylene-chloride, and the organic layers were washed twice with 1 N NaOH, once with H2O
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated to dryness under reduced pressure
  7. customto yield a colorless oil
  8. customto give colorless crystals, mp 27°-28°