HRID553261

反应详情

EQUATION

反应方程式

HRID 553261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5-dihydroxyacetophenone (5.00 g, 0.0329 mol), benzyl bromide (3.72 ml, 0.031 mol), potassium carbonate (4.31 g, 0.031 mol) and acetone (150 ml) were added to a 500 ml round bottom flask. The reaction mixture was heated overnight at reflux and then was cooled to ambient temperature. When cool, deionized water (150 ml) was added to the reaction mixture and the reaction mixture was extracted three times with 100 ml portions of diethyl ether. The combined ether layers were dried with sodium sulfate and concentrated in vacuo yielding a dark solid. This dark solid was recrystallized from 50:50 (ethanol:water) yielding 3.09 g of 2-hydroxy-5-benzyloxyacetophenone as yellow needles.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated overnight
  2. temperatureat reflux
  3. temperatureWhen cool
  4. extractionthe reaction mixture was extracted three times with 100 ml portions of diethyl ether
  5. dry with materialThe combined ether layers were dried with sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customyielding a dark solid
  8. customThis dark solid was recrystallized from 50:50 (ethanol:water)