反应详情

11 g (25 mmol) of methyl 3-benzyloxy-3-phenyl-2-hydroxybutyrate (compound 1.1) are dissolved in 50 ml of dichloromethane, 3 g (30 mmol) of triethylamine are added and 3.2 g (28 mmol) of methanesulfonyl chloride are added dropwise while stirring. Stirring is continued for 2 hours at room temperature, and the mixture is washed with water, dried over magnesium sulfate and evaporated down under reduced pressure. The residue is taken up in dimethylformamide and the solution is added dropwise at 0° C. to a suspension of 12.9 g (75 mmol) of 4,6-dimethoxypyrimidine-2-thiol and 8.4 g (100 mmol) of sodium bicarbonate in 100 ml of dimethylformamide. After stirring has been carried out for 2 hours at room temperature and for a further 2 hours at 60° C., the mixture is poured onto 11 of ice water and the resulting precipitate is filtered off with suction. After drying, 3.2 g of a white powder remain.

1. stirringStirring
2. washthe mixture is washed with water
3. dry with materialdried over magnesium sulfate
4. customevaporated down under reduced pressure
5. stirringAfter stirring
6. waithas been carried out for 2 hours at room temperature and for a further 2 hours at 60° C.
7. filtrationthe resulting precipitate is filtered off with suction
8. customAfter drying