反应详情

温度

140 °C

370 mg (14.7 mmol) sodium hydride was given to a solution of 2.31 g (13.3 mmol) 2-chloro-4-nitrophenol in 25 ml DMF. Stirring was continued for 30 min. at room temperature. 2.50 g (13.3 mmol) 3-(4-Chloro-pyrimidin-2-ylamino)-propan-1-ol were added and the mixture heated to 140° C. for 24 h. The reaction mixture was evaporated, taken up with water and extracted with dichloromethane. The organic phase was extracted with sodium carbonate solution, dried (sodium sulphate) and evaporated. The obtained material was dissolved in 3 ml dichloromethane and purified by chromatography over silica (dichloromethane/ethanol 95:5) to give 2.92 g (67%) 3-[4-(2-chloro-4-nitro-phenoxy)-pyrimidin-2-ylamino]-propan-1-ol.

1. customThe reaction mixture was evaporated
2. extractionextracted with dichloromethane
3. extractionThe organic phase was extracted with sodium carbonate solution
4. dry with materialdried (sodium sulphate)
5. customevaporated
6. dissolutionThe obtained material was dissolved in 3 ml dichloromethane
7. custompurified by chromatography over silica (dichloromethane/ethanol 95:5)