HRID536012
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customReaction mixture
- temperaturewas cooled to 20-25° C
- concentrationIt was then concentrated under vacuum
- dissolutionThe residue was dissolved in water (50 ml)
- customprecipitated solid
- filtrationwas filtered off
- customThe solid obtained
- customwas further purified by column chromatography