反应详情

A solution of 16.8 g (40 mmol) 2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine, 7.35 g 4-nitro-2,5-dimethylphenol (44 mmol) and 8.29 g potassium carbonate (60 mmol) in 70 ml DMF were stirred for 20 hrs at 100° C. After adding the mixture to 150 ml water the resulting suspension was extracted twice with 50 ml dichloromethane. The combined organic layers were washed with aqueous solution of sodium hydroxide. The organic layer was dried over magnesium sulfate, concentrated in vacuo and column chromatography (dichloromethane) yielded 8.3 g (47%) with a purity of 76%; log P (pH=2.3)=4.07.

1. extractionwas extracted twice with 50 ml dichloromethane
2. washThe combined organic layers were washed with aqueous solution of sodium hydroxide
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationconcentrated in vacuo and column chromatography (dichloromethane)
5. customyielded 8.3 g (47%) with a purity of 76%