反应详情

7.16 g (25 mmol) of methyl 2-hydroxy-3-methoxy-3,3-diphenylpropionate were dissolved in 50 ml of dichloromethane, 3 g (30 mmol) of triethylamine were added, and 3.2 g (28 mmol) of methane-sulfonyl chloride were added dropwise while stirring. The mixture was stirred at room temperature for 2 h., washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was taken up in DMF and 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 DMF. After stirring at room temperature for 2 h. and at 60° C. for a further 2 h., the mixture was poured into 1 liter of ice-water, and the resulting precipitate was filtered off with suction. After drying, 3.19 g (29%) of a white powder remained.

1. stirringThe mixture was stirred at room temperature for 2 h.
2. washwashed with water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. stirringAfter stirring at room temperature for 2 h. and at 60° C. for a further 2 h.
6. filtrationthe resulting precipitate was filtered off with suction
7. customAfter drying