HRID1926584

反应详情

EQUATION

反应方程式

HRID 1926584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chloro-N6-cyclopentyladenosine-2′,3′,5′-triacetoxy-2,6-dichloroadenosine (1.5 g) and cyclopentylamine (8 eq.) were diluted with ethanol (50 eq.) and the resulting solution was heated at reflux for about 15 hours, then cooled to room temperature and concentrated in vacuo to provide a crude residue which was diluted with a mixture of ethyl acetate and water and transferred to a separatory funnel. The organic layer was separated, dried over sodium sulfate and concentrated in vacuo to provide a crude residue which was purified using flash column chromatography on silica gel (8% MeOH—dichloromethane as eluent) to provide 2-chloro-N6-cyclopentyladenosine (0.948 g). MS m/z 370.32 [M+H]+.

WORKUP

后处理

  1. temperaturethe resulting solution was heated
  2. temperatureat reflux for about 15 hours
  3. concentrationconcentrated in vacuo
  4. customto provide a crude residue which
  5. customtransferred to a separatory funnel
  6. customThe organic layer was separated
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in vacuo
  9. customto provide a crude residue which
  10. customwas purified