HRID275343

反应详情

EQUATION

反应方程式

HRID 275343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2,6-dichloropurine (0.30 g, 1.6 mmol) is added to a mixture of benzyl alcohol (0.19 g, 1.8 mmol) and 60% sodium hydride (0.13 g, 3.3 mmol) in DMF (8 ml) at room temperature (RT). After 1 hr, the reaction is heated to 60° C. for 18 hr, cooled to RT and dilute HCl is added to adjust the pH to 5. The mixture is extracted with EtOAc/THF 1:1, and the organic layer is dried over sodium sulfate, filtered and concentrated to give a solid. This is recrystallized from EtOAc/hexane to give the title compound, mp. 195°-196° C.

WORKUP

后处理

  1. temperaturecooled to RT
  2. extractionThe mixture is extracted with EtOAc/THF 1:1
  3. dry with materialthe organic layer is dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give a solid
  7. customThis is recrystallized from EtOAc/hexane