反应详情

48.5 g (161.55 mmol) of 6-(2,4-dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine (Example 3A) and 163.84 g (969.32 mmol) of bromoacetaldehyde dimethyl acetal are introduced into a mixture of 1164 ml of dioxane and 291 ml of water and heated under reflux for 16 h. The dioxane is substantially removed in vacuo, and 1000 ml of ethyl acetate and 1000 ml of saturated aqueous sodium bicarbonate solution are cautiously added. The phases are separated and a further extraction with ethyl acetate is carried out. The combined organic phases are washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and then freed of solvent. The residue is purified by silica gel chromatography. 16.6 g (27% of theory) of the product are obtained and are reacted further in this form.

1. temperatureheated
2. temperatureunder reflux for 16 h
3. customThe dioxane is substantially removed in vacuo, and 1000 ml of ethyl acetate and 1000 ml of saturated aqueous sodium bicarbonate solution
4. additionare cautiously added
5. customThe phases are separated
6. extractiona further extraction with ethyl acetate
7. washThe combined organic phases are washed with saturated aqueous sodium chloride solution
8. dry with materialdried over sodium sulphate
9. customThe residue is purified by silica gel chromatography
10. custom16.6 g (27% of theory) of the product are obtained
11. customare reacted further in this form