反应详情

温度

140 °C

Cesium carbonate was added to a solution of 2-Amino-4-(2,4-dichloro-5-hydroxyphenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in DMF, 2-Bromo-N,N-diethylethylamine hydrobromide was added and the suspension heated, at ˜140° C., for ˜2 hrs. The resulting suspension was allowed to cool and dichloromethane added. The mixture was washed with water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a dark brown gum. The crude product was purified by chromatography on silica eluting with mixtures of dichloromethane and methanol.

1. additionwas added
2. temperatureto cool
3. washThe mixture was washed with water and saturated aqueous sodium chloride solution
4. dry with materialThe solution was dried over anhydrous sodium sulphate
5. concentrationconcentrated to a dark brown gum
6. customThe crude product was purified by chromatography on silica eluting with mixtures of dichloromethane and methanol