HRID323873

反应详情

EQUATION

反应方程式

HRID 323873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.6 g (18.72 mmol) of potassium carbonate were added at 60° C. to a suspension of 3.0 g (11.7 mmol) of 7-benzyl-3-methylxanthine (prepared according to Example 1a) in 70 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 3.1 g (15.21 mmol) of 2-phenoxyethyl bromide were then added dropwise and the mixture was stirred at 80° C. for 5 hours. The crude mixture was then filtered, the filtrate was concentrated under reduced pressure, the residue was taken up in dichloromethane and the solution was washed once with 1 N sodium hydroxide solution and twice with water. The organic phases were dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (1/2).

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. for 5 hours
  2. filtrationThe crude mixture was then filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. washthe solution was washed once with 1 N sodium hydroxide solution and twice with water
  5. customThe organic phases were dried
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (1/2)