HRID1492833

反应详情

EQUATION

反应方程式

HRID 1492833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.90 g (5.3 mmol) of 3,5-dihydroxybenzoic acid methyl ester, 2.95 g (11.8 mmol) of 2-(2-bromoethoxy)naphthalene, 1.8 g (11.8 mmol) of sodium iodide and 3 g (21.7 mmol) of potassium carbonate in 80 mL of acetone and 25 mL of DMF was stirred at reflux for 40 hours. The solvents were removed at reduced pressure, water was added to the residue and the product was extracted with ethyl acetate. The dried extract was concentrated to a solid which was recrystallized from ethyl acetate to give 1.6 g (59% yield, mp 132°-137°) of 3,5-bis[2-[2-(naphthalenyloxy) ethoxy]benzoic acid methyl ester.

WORKUP

后处理

  1. temperatureat reflux for 40 hours
  2. customThe solvents were removed at reduced pressure, water
  3. additionwas added to the residue
  4. extractionthe product was extracted with ethyl acetate
  5. extractionThe dried extract
  6. concentrationwas concentrated to a solid which
  7. customwas recrystallized from ethyl acetate