反应详情

3,6-dichlorobenzisoxazole (5.2 g, 27.8 mmol), and anhydrous piperazine (24 g, 278 mmol) are placed in an egg type flask and react at 120° C. for 24 hours. After completion of the reaction, 52 ml of an ice-water mixture is added for quenching the reaction. Further 15 ml of 50% NaOH solution is added to the reaction solution. The reaction solution is stirred for 5 minutes and extracted with dichloromethane (30 ml×3). The dichloromethane layer is combined, washed with 20 ml of saturated saline, dried over anhydrous MgSO4, evaporated to dryness, and subjected to a separation on a column of alumina (200-300 mesh), eluting with dichloromethane:methanol-100:1, to obtain 4.7 g of 6-chloro-3-piperazinyl-benzisoxazole, with a yield of 71%.

1. customreact at 120° C. for 24 hours
2. additionis added
3. customfor quenching
4. customthe reaction
5. extractionextracted with dichloromethane (30 ml×3)
6. washwashed with 20 ml of saturated saline
7. dry with materialdried over anhydrous MgSO4
8. customevaporated to dryness
9. customsubjected to a separation on a column of alumina (200-300 mesh)
10. washeluting with dichloromethane