反应详情

7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone (297 mg, 1 mmol), 3-(4-piperidinyl)-1,2-benzisothiazole (220 mg, 1 mmol), and anhydrous potassium carbonate powder (414 mg, 3.3 mmol) are added to 10 ml and react at reflux for 24 hours. The reaction solution is evaporated to dryness and dispersed with 20 ml of dichloromethane and 20 ml of water respectively. The organic layer is extracted with water (20 ml×2) and saturated saline (20 ml) successively, dried over anhydrous magnesium sulfate, and evaporated to dryness to obtain a light yellow powder, which is dissolved into 5 ml of acetone and stirred in an ice bath to precipitate a white solid. The white solid is filtered, washed with small amount of acetone, and dried to obtain 260 mg of a whiter powder. The whiter powder is dissolved into anhydrous ethanol and thereto is drop-added HCl/EtOH to adjust to pH=2 to precipitate a white deposit, which is filtered out and recrystallized in anhydrous ethanol to obtain 200 mg of a product, with a yield of 44%.

1. customreact
2. temperatureat reflux for 24 hours
3. customThe reaction solution is evaporated to dryness
4. additiondispersed with 20 ml of dichloromethane and 20 ml of water respectively
5. extractionThe organic layer is extracted with water (20 ml×2) and saturated saline (20 ml) successively
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated to dryness
8. customto obtain a light yellow powder, which
9. customto precipitate a white solid
10. filtrationThe white solid is filtered
11. washwashed with small amount of acetone
12. customdried
13. customto obtain 260 mg of a whiter powder
14. customto precipitate a white deposit, which
15. filtrationis filtered out
16. customrecrystallized in anhydrous ethanol