HRID925559

反应详情

EQUATION

反应方程式

HRID 925559 的结构方程式

CONDITIONS

反应条件

温度
127.5 °C

PROCEDURE

实验过程

A mixture of 1-Propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-3,7-dihydro-purine-2,6-dione (0.2 g, 0.45 mmol), POCl3 (5 ml) and NH4Cl (0.486 g, 9 mmol) were heated at 125-130° C. for 20 hours. Reaction mixture was cooled to 20-25° C. It was then concentrated under vacuum. The residue was dissolved in water (50 ml) and precipitated solid was filtered off. The solid obtained was further purified by column chromatography to obtain pure 2-Chloro-1-propyl-8-[6-(3-trifluoromethyl-benzylamino)-pyridin-3-yl]-1,7-dihydro-purin-6-one as pale yellow solid (0.054 g, 26%).

WORKUP

后处理

  1. customReaction mixture
  2. temperaturewas cooled to 20-25° C
  3. concentrationIt was then concentrated under vacuum
  4. dissolutionThe residue was dissolved in water (50 ml)
  5. customprecipitated solid
  6. filtrationwas filtered off
  7. customThe solid obtained
  8. customwas further purified by column chromatography