反应详情

温度

150 °C

To a sealed tube was added 4methoxy-benzo[d]isothiazole (760 mg, 4.60 mmol) and pyridine hydrochloride (5.5 g, 48 mmol). The reaction was heated to 150° C. for 18 h and was then cooled to rt. The mixture was partitioned between dichloromethane and water. The organic phase was separated and the aqueous layer was extracted with 2×30 mL dichloromethane. The combined organic phases were dried (MgSO4) and concentrated in vacuo. The residue was purified by flash chromatography eluting silica gel with EtOAc:hexane [0:100 to 3:7] to yield the title compound as a solid (223 mg, 32%); Mass spectrum (ion spray): m/z=151.9 (m+1).

1. temperaturewas then cooled to rt
2. customThe mixture was partitioned between dichloromethane and water
3. customThe organic phase was separated
4. extractionthe aqueous layer was extracted with 2×30 mL dichloromethane
5. dry with materialThe combined organic phases were dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography
8. washeluting silica gel with EtOAc