HRID1389244

反应详情

EQUATION

反应方程式

HRID 1389244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.45 g (0.07 mole) of adenine are added to a solution of 1.6 g (0.07 mole) of sodium in 250 ml of isopropanol and the reaction mixture heated under reflux for 10 minutes. It is then cooled and 21.4 g (0.08 mole) of 3-(4-phenoxymethylpiperidino)-propyl chloride in 50 ml of isopropanol added thereto. After stirring the reaction mixture under reflux for 6 hours, it is evaporated in a vacuum, the residue is taken up in methylene chloride, the methylene chloride solution is washed with 2 N aqueous sodium hydroxide solution and subsequently with water, dried over anhydrous sodium sulfate, evaporated and the residue recrystallized from isopropanol. There are obtained 16.4 g (64% of theory) of 9-[3-(4-phenoxymethylpiperidino)-propyl]-adenine; m.p. 142°-144° C.

WORKUP

后处理

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 10 minutes
  3. temperatureIt is then cooled
  4. temperatureunder reflux for 6 hours
  5. customit is evaporated in a vacuum
  6. washthe methylene chloride solution is washed with 2 N aqueous sodium hydroxide solution and subsequently with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated
  9. customthe residue recrystallized from isopropanol