反应详情

6-Methoxy-N-[2-(4-morpholinyl)ethyl]-1,2-benzisoxazol-3-amine (2.9 g) was dissolved in 48% hydrobromic acid (50 ml) and heated to reflux under nitrogen for 3 hours. The reaction was cooled to room temperature, neutralized with saturated sodium carbonate (Na2CO3) solution, and extracted with EtOAc. The organic phase was dried over MgSO4 and concentrated in vacuo. Flash chromatography (silica gel) eluting with 3:2 acetone/heptane and subsequently titration with DCM/heptane provided the product (1.0 g), m.p. 151-152° C.

1. temperatureheated
2. temperatureto reflux under nitrogen for 3 hours
3. extractionextracted with EtOAc
4. dry with materialThe organic phase was dried over MgSO4
5. concentrationconcentrated in vacuo
6. washFlash chromatography (silica gel) eluting with 3:2 acetone/heptane and subsequently titration with DCM/heptane