HRID273278

反应详情

EQUATION

反应方程式

HRID 273278 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

17.92 g (0.1 mole) of 2-amino-9-(2-hydroxyethyl)purine was completely dissolved in 400 ml of acetonitrile, to which 84.42 g (0.20 mole) of dibromotriphenylphosphine was then added. The mixture was stirred for 5 hours at a temperature of 30-40° C. After completion of the reaction, 300 ml of water was added to the reaction product. The resulting solution was neutralized with aqueous sodium hydroxide solution and extracted four times with 500 ml portions of a mixed solution of chloroform and methanol (4:1). The organic layer was collected, and dried with anhydrous magnesium sulfate, followed by filtration and washing. The resulting filtrate was concentrated under reduced pressure, and crystallized from chloroform, 22.03 g (91%) of white 2-amino-9-(2-bromoethyl)purine.

WORKUP

后处理

  1. additionwas then added
  2. additionwas added to the reaction product
  3. extractionextracted four times with 500 ml portions of a mixed solution of chloroform and methanol (4:1)
  4. customThe organic layer was collected
  5. dry with materialdried with anhydrous magnesium sulfate
  6. filtrationfollowed by filtration
  7. washwashing
  8. concentrationThe resulting filtrate was concentrated under reduced pressure
  9. customcrystallized from chloroform, 22.03 g (91%) of white 2-amino-9-(2-bromoethyl)purine