HRID2165815

反应详情

EQUATION

反应方程式

HRID 2165815 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Methyl-7-propylxanthine (10.4 g) was dissolved in 200 ml of an ethanol/water (3:2 (v/v)) mixed solution containing 2.2 g of sodium hyddroxide and 15.5 g of 4-(4-methoxyphenoxy)butylbromide was added to the solution. The mixture was then refluxed at elevated temperatures for 12 hours. The reaction mixture was concentrated under reduced pressure to give the residual liquid which in turn was alkalized with 1N-sodium hydroxide solution and then extracted with chloroform. The extract was dried and concentrated under reduced pressure to dryness. The residue was then subjected to silica gel column chromatography using a chloroform/ethanol (40:1 (v/v)) eluent to yield 12.5 g (65%) of 1-[4-(4-methoxyphenoxy)butyl]-3-methyl-7-propylxanthine.

WORKUP

后处理

  1. additionmixed solution
  2. additionwas added to the solution
  3. temperatureThe mixture was then refluxed at elevated temperatures for 12 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. customto give the residual liquid which in turn
  6. extractionextracted with chloroform
  7. customThe extract was dried
  8. concentrationconcentrated under reduced pressure to dryness