HRID1863304

反应详情

EQUATION

反应方程式

HRID 1863304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

To a solution of 5.0 g of p-benzyloxyphenol and 1.19 g of sodium methoxide in 40 ml of methanol is added 50 mg of potassium iodide and 7.11 g of methyl α-bromo-α-[p-(p-chlorophenoxy)phenyl]acetate in 10 ml of benzene. The mixture is refluxed for 22 hours and poured into ice and water. The mixture is extracted with ether and the ether extracts washed with 10% potassium carbonate and with water. The extracts are dried (MgSO4) and the solvent removed under vacuum to give an oily solid. Trituration with hexane plus a small amount of acetone and chilling gives crystals. Filtration gives the product as off-white crystals, mp 91°-96° C. Recrystallization by dissolving in hot acetone, diluting with petroleum ether, chilling and filtering gives the product as white crystals, mp 88°-90° C.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 22 hours
  2. extractionThe mixture is extracted with ether
  3. washthe ether extracts washed with 10% potassium carbonate and with water
  4. dry with materialThe extracts are dried (MgSO4)
  5. customthe solvent removed under vacuum
  6. customto give an oily solid
  7. customgives crystals
  8. filtrationFiltration