反应详情

温度

60 °C

To 300 mg (0.766 mmol) of N-4-(l-methoxy-1-buten-4-yl)benzoyl-L-glutamic acid diethyl ester, 3.0 ml of acetonitrile, and 3.0 ml of water, stirred at room temperature, are added 122 mg (0.766 mmol) of bromine in 1 ml of acetonitrile. To this solution is added 188 mg (2.3 mmol) of sodium acetate and 0.97 mg (0.77 mmol) of 2,4-diamino-6-hydroxypyrimidine and the resulting mixture is heated to 60° C. for 18 hours, cooled, then concentrated under vacuum. The resulting residue is triturated (2×5 ml of water) and decanted. Ethanol (5 ml) and 440 mg (2.3 mmol) of p-toluenesulfonic acid monohydrate are added. After heating under reflux for 20 minutes the mixture is cooled to room temperature and filtered. The precipitate is washed with ethanol (2×5ml) and dried to obtain a p-toluenesulfonate salt of the title compound.

1. temperaturecooled
2. concentrationconcentrated under vacuum
3. customThe resulting residue is triturated (2×5 ml of water)
4. customdecanted
5. temperatureAfter heating
6. temperatureunder reflux for 20 minutes the mixture
7. temperatureis cooled to room temperature
8. filtrationfiltered
9. washThe precipitate is washed with ethanol (2×5ml)
10. customdried