反应详情

温度

140 °C

To a sealed tube was added 3-chloro-6-methoxy-1,2-benzisoxazole (3.0 g) and piperazine (6.0 g). The reaction was heated to 140° C. over 4 hours and then cooled to room temperature. The residue was dissolved in MeOH and further diluted with EtOAc (11). The precipatate was filtered and the filtrate dried over MgSO4 and concentrated in vacuo. Flash chromatography (silica gel) eluting with 30% MeOH/EtOAc provided a residue upon evaporation (3.6 g), m.p. 79°-80° C.

1. temperaturecooled to room temperature
2. filtrationThe precipatate was filtered
3. dry with materialthe filtrate dried over MgSO4
4. concentrationconcentrated in vacuo
5. washFlash chromatography (silica gel) eluting with 30% MeOH/EtOAc
6. customprovided a residue
7. customupon evaporation (3.6 g), m.p. 79°-80° C.