反应详情

Potassium tert-butoxide was added to a suspension of 2-Amino-4-(2,4-dichloro-5-hydroxyphenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in acetonitrile, bromoacetaldehyde diethyl acetal was added and the suspension heated under reflux for ˜8 hrs. The resulting suspension was allowed to cool and water added, the mixture was extracted with ethyl acetate and the extracts washed with water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a red/brown gum. The crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane.

1. additionwas added
2. temperaturethe suspension heated
3. temperatureunder reflux for ˜8 hrs
4. temperatureto cool
5. extractionthe mixture was extracted with ethyl acetate
6. washthe extracts washed with water and saturated aqueous sodium chloride solution
7. dry with materialThe solution was dried over anhydrous sodium sulphate
8. concentrationconcentrated to a red/brown gum
9. customThe crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane