反应详情

温度

80 °C

A mixture of 5-bromo-1,3,4-thiadiazol-2-ylamine, K2HPO4 (5.7 g), and 5.3 ml of morpholine in 20 ml of DMF is heated at 80° C. under nitrogen for 18 hours, then diluted with 50 ml of water. The clear solution is placed in a continuous extractor and extracted with a brisk flow of dichloromethane for 18 hours. The solution is dried over MgSO4 and concentrated under reduced pressure, with toluene azeotropes to remove DMF. Recrystallization of the residual solid from 50 ml of acetonitrile and 100 ml of toluene affords 3.92 g of the title compound.

1. extractionextracted with a brisk flow of dichloromethane for 18 hours
2. dry with materialThe solution is dried over MgSO4
3. concentrationconcentrated under reduced pressure, with toluene azeotropes
4. customto remove DMF
5. customRecrystallization of the residual solid from 50 ml of acetonitrile and 100 ml of toluene