反应详情

温度

140 °C

A mixture of 3-chloro-6-methoxy-1,2-benzisoxazole (3.0 g) and piperazine (6.0 g) was heated to 140° C. over 4 hours in a sealed tube and then cooled to room temperature. The contents of the tube were dissolved in MeOH and further diluted with EtOAc (1 L). The precipitate 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 precipitate 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.)