反应详情

温度

140 °C

To a sealed tube was added 7-bromo-3-chloro-6-methoxy-1,2-benzisoxazole (2.0 g) and piperazine (2.6 g). The reaction was heated to 140° C. over 30 minutes and then cooled to room temperature. The residue was dissolved in MeOH and concentrated in vacuo. Flash column chromatography (silica gel) eluting with 30% MeOH/EtOAc provided a residue upon evaporation (1.0 g) which was recrystallized from MeOH/CH2Cl2 /pet. ether to yield 1.0 g, m.p. 268-269° C.

1. temperaturecooled to room temperature
2. concentrationconcentrated in vacuo
3. washFlash column chromatography (silica gel) eluting with 30% MeOH/EtOAc
4. customprovided a residue
5. customupon evaporation (1.0 g) which
6. customwas recrystallized from MeOH/CH2Cl2 /pet. ether
7. customto yield 1.0 g, m.p. 268-269° C.