HRID1981993

反应详情

EQUATION

反应方程式

HRID 1981993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an argon atmosphere, 2 g of [(8-acetyl-7-hydroxy-2-naphthalenyl)oxy]acetic acid methyl ester was added to a suspension of 0.32 g of 60% sodium hydride in 30 ml of anhydrous dimethylformamide. The mixture was stirred at room temperature for 40 minutes and then 11.6 g of bis[2-[2-bromoethoxy)ethyl]ether was added and the mixture was stirred at room temperature for 20 hours. The resulting dark mixture was concentrated in vacuo to an oil which was dissolved in methylene chloride, washed with water and concentrated to give an oil. Purification by high pressure liquid chromatography (35% ethyl acetate-toluene) gave 3.0 g (80%) of [[8-acetyl-7-[2-[2-[2-(2-bromoethoxy)ethoxy]ethoxy]ethoxy]-2-naphthalenyl]oxy]acetic acid methyl ester as an oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 20 hours
  2. concentrationThe resulting dark mixture was concentrated in vacuo to an oil which
  3. dissolutionwas dissolved in methylene chloride
  4. washwashed with water
  5. concentrationconcentrated
  6. customto give an oil
  7. customPurification by high pressure liquid chromatography (35% ethyl acetate-toluene)