HRID1011177

反应详情

EQUATION

反应方程式

HRID 1011177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(Butyloxy)-8-(methoxy)-9-(tetrahydro-3-furanylmethyl)-9H-purin-6-amine (Isomer 1, 1.54 gm) was suspended in methanol (20 ml) and 4N HCl in dioxan (4 ml) added with stirring to give a clear solution. After 6.5 h, the solvents were evaporated to low volume and water added with stirring, followed by neutralisation with saturated sodium bicarbonate. The resulting off-white solid was filtered, washed with water and dried, yield 1.26 gm. This material was added portionwise to boiling methanol (130 ml), adding a further 20 ml of methanol. The suspension was filtered, and the solid treated with boiling methanol (20 ml) and added to the filtrate. This was reboiled, then allowed to cool with stirring when a white solid crystallised out. This was filtered, washed with methanol and dried, to give the title compound yield 932 mg.

WORKUP

后处理

  1. customto give a clear solution
  2. customthe solvents were evaporated to low volume and water
  3. additionadded
  4. stirringwith stirring
  5. filtrationThe resulting off-white solid was filtered
  6. washwashed with water
  7. customdried
  8. additionThis material was added portionwise
  9. additionadding a further 20 ml of methanol
  10. filtrationThe suspension was filtered
  11. additionthe solid treated with boiling methanol (20 ml)
  12. additionadded to the filtrate
  13. temperatureto cool
  14. stirringwith stirring when a white solid
  15. customcrystallised out
  16. filtrationThis was filtered
  17. washwashed with methanol
  18. customdried