HRID1981985

反应详情

EQUATION

反应方程式

HRID 1981985 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, 1 g of [(8-acetyl-7-hydroxy-2-naphthalenyl)oxy]acetic acid methyl ester was added to a suspension of 0.16 g of 60% sodium hydride in 15 ml of anhydrous dimethylformamide. The mixture was stirred at room temperature for 40 minutes and then 4.75 g of bis(3-bromopropyl)ether was added. The mixture was stirred at room temperature for 20 hours. The mixture was concentrated in vacuo to an oil which was dissolved in ethyl acetate, washed with water and concentrated to give an oil which was purified by column chromatography using 7.5% ethyl acetate-toluene to yield 1 g (60%) of [[8-acetyl-7-[3-(3-bromopropoxy)propoxy]-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 mixture was concentrated in vacuo to an oil which
  3. dissolutionwas dissolved in ethyl acetate
  4. washwashed with water
  5. concentrationconcentrated
  6. customto give an oil which
  7. customwas purified by column chromatography