反应详情

5.9 g (25 mmol) of methyl 3-azido-3-phenyl-2-hydroxybutyrate (Ex. 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 with stirring. The mixture is stirred for 23 hours at room temperature, washed three times with 100 ml of water each time, dried over sodium sulfate and concentrated under reduced pressure. The residue is taken up in 100 ml of 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 hydrogencarbonate in 100 ml of DMF. After stirring at room temperature for 2 hours and at 60° C. for a further 2 hours, the mixture is poured onto 1 l of ice water and the resulting precipitate is filtered off with suction.

1. stirringThe mixture is stirred for 23 hours at room temperature
2. washwashed three times with 100 ml of water each time
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. stirringAfter stirring at room temperature for 2 hours and at 60° C. for a further 2 hours
6. filtrationthe resulting precipitate is filtered off with suction