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温度

0 °C

Preparation: 30 g of Naproxen chloride are dissolved in 120 g of dichloromethane. This solution is cooled at 0° C. and a solution of 14.5 g of 1-chloro-3-buthanol in 100 g of dichloromethane is added dropwise in 2 hours. After a completion time of 3 hours at 0° C., 60 g of water are added and is the mixture is stirred for 10 hours. After phase separation, 60 g of water are added to organic phase and the mixture is stirred for 10 hours. After phase separation, the organic phase is concentrated to 120 mL and 4.5 g of potassium carbonate are added. The mixture is refluxed at about 40° C. for 4 hours. After filtration and vacuum concentration, an oil is obtained (HPLC purity 90%).

1. customPreparation
2. customAfter phase separation, 60 g of water
3. additionare added to organic phase
4. stirringthe mixture is stirred for 10 hours
5. customAfter phase separation
6. concentrationthe organic phase is concentrated to 120 mL and 4.5 g of potassium carbonate
7. additionare added
8. temperatureThe mixture is refluxed at about 40° C. for 4 hours
9. filtrationAfter filtration and vacuum concentration
10. customan oil is obtained (HPLC purity 90%)