反应详情

A mixture of 5.0 g of 3-(4-piperidinyl)-1,2-benzisothiazole, 7.70 g of 4-chloro-1,1-bis(4-fluorophenyl)butane, 7.0 g of potassium carbonate, 0.25 g of potassium iodide and 120 ml of dimethylformamide was stirred at 90° for 8.0 hrs and overnight at ambient temperature. The reaction mixture was poured into water, extracted with ethyl acetate, washed with water, dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to yield an oil. The product was purified by high-pressure liquid chromatography using dichloromethane:methanol (2%) as the eluent. The eluent was evaporated, the residue was dissolved in ether and a saturated hydrogen chloride/ether solution was added dropwise to yield a solid. The solid was recrystallized from ethyl acetate/ether to give 2.0 g (21%) of product, mp 198°-199°.

1. extractionextracted with ethyl acetate
2. washwashed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was removed in vacuo
5. customto yield an oil
6. customThe product was purified by high-pressure liquid chromatography
7. customThe eluent was evaporated
8. dissolutionthe residue was dissolved in ether
9. additiona saturated hydrogen chloride/ether solution was added dropwise
10. customto yield a solid
11. customThe solid was recrystallized from ethyl acetate/ether