反应详情

温度

80 °C

160 mg (6.34 mmol) 95% sodium hydride was given to a solution of 1.00 g (5.76 mmol) 3-chloro-4-nitrophenol in 15 ml DMF. Stirring was continued for 30 min. at room temperature. 925 mg (5.76 mmol) 4-chloro-2-methylsulfanyl-pyrimidine was added and the mixture heated to 80° C. for 16 h. The reaction mixture was evaporated, taken up with water and extracted with ethyl acetate. The organic phase was extracted with water, dried (sodium sulphate) and evaporated. The obtained material was dissolved in ethyl acetate and purified by chromatography over silica (ethyl acetate/n-heptane) to give 1.10 g (64%) 4-(3-chloro-4-nitro-phenoxy)-2-methylsulfanyl-pyrimidine.

1. customThe reaction mixture was evaporated
2. extractionextracted with ethyl acetate
3. extractionThe organic phase was extracted with water
4. dry with materialdried (sodium sulphate)
5. customevaporated
6. dissolutionThe obtained material was dissolved in ethyl acetate
7. custompurified by chromatography over silica (ethyl acetate/n-heptane)