反应详情

1.8 g [11 mmol] of 3-amino-4-methoxy-1,2-benzisoxazole and 22.5 g [151.8 mmol] of triethyl orthoformate are boiled under reflux with exclusion of moisture for 18 hours. After concentrating by rotary evaporation under reduced pressure, the remaining residue is taken up in 50 ml of ethanol and, after the addition of 3.05 g [80.6 mmol] of sodium borohydride, the mixture is stirred first at room temperature for 3 hours and then at 50° C. for 12 hours. The mixture is concentrated, and the residue is dissolved in dichloromethane and washed with water. After drying and concentrating the organic phase, 1.5 g of the compound (XIIa-1) are obtained as a white solid.

1. temperatureunder reflux with exclusion of moisture for 18 hours
2. concentrationAfter concentrating by rotary evaporation under reduced pressure
3. waitat 50° C. for 12 hours
4. concentrationThe mixture is concentrated
5. dissolutionthe residue is dissolved in dichloromethane
6. washwashed with water
7. customAfter drying
8. concentrationconcentrating the organic phase, 1.5 g of the compound (XIIa-1)
9. customare obtained as a white solid