反应详情

温度

52.5 °C

Finely ground NaBH4 (1 g) is added to a solution of 6,7-dichloro-4-cyclopropyl-4H-1,2,4-benzothiadiazine 1,1-dioxide from the Step above (1.9 g) in isopropanol (50 mL) and then heated at 50-55° C. for 5-10 minutes. The solvent is removed by evaporation under reduced pressure. The residue is taken up in water (50 mL) and brought to acid pH by adding 6N HCl. The title product is extracted with dichloromethane (3×30 mL). The organic phase is dried over MgSO4 and filtered. The filtrate is evaporated to dryness and the residue obtained is recrystallised from methanol/water 1/1 (60 mL).

1. customThe solvent is removed by evaporation under reduced pressure
2. additionby adding 6N HCl
3. extractionThe title product is extracted with dichloromethane (3×30 mL)
4. dry with materialThe organic phase is dried over MgSO4
5. filtrationfiltered
6. customThe filtrate is evaporated to dryness
7. customthe residue obtained
8. customis recrystallised from methanol/water 1/1 (60 mL)