HRID2297655

反应详情

EQUATION

反应方程式

HRID 2297655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (3aS,4S,6R,6aR)-6-(6-chloro-purin-9-yl)-2,2-dimethyl-tetrahydro-furo[3,4-d][1,3]dioxole-4-carboxylic acid (5.82 g) and isopropyl amine (7.27 ml) in isopropanol (20 ml) was heated under reflux for 40 h, cooled to room temperature and concentrated in vacuo. The resulting residue was partitioned between ethyl acetate (75 ml) and citric acid (0.5M, 75 ml). The layers were separated, and the organic phase washed with citric acid solution (2×50 ml). The combined organic extracts were washed with water (50 ml) and brine (80 ml), dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a light brown foam (4.49 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 40 h
  3. concentrationconcentrated in vacuo
  4. customThe resulting residue was partitioned between ethyl acetate (75 ml) and citric acid (0.5M, 75 ml)
  5. customThe layers were separated
  6. washthe organic phase washed with citric acid solution (2×50 ml)
  7. washThe combined organic extracts were washed with water (50 ml) and brine (80 ml)
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo