Reaktion #93150

Reaktionsgleichung

potassium iodide

4-phenylpiperazine

3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole

sodium bicarbonate

dimethylformamide

→

1-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-phenylpiperazine oxalate

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe mixture was filtered
2. 2
   Sonstigethe filtrate was evaporated to an oil
3. 3
   workup.STIRRINGThe oil was stirred with 100 ml of water for five mins
4. 4
   Extraktionextracted with ether
5. 5
   ExtraktionThe ether extract
6. 6
   Waschenwas washed with water (2×), saturated sodium chloride solution
7. 7
   Trocknendried over anhydrous magnesium sulfate
8. 8
   FiltrationAfter filtering
9. 9
   SonstigeRecrystallization twice from ethyl acetate/methanol/ether
10. 10
    Sonstigeyielded the analytical sample mp 188°-190° C. (dec)

Vorschrift

To 35 ml of dry dimethylformamide was added 1.6 g of 4-phenylpiperazine, 2.1 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 8.0 g of sodium bicarbonate, and a few crystals of potassium iodide. The mixture was heated at 100° C. for three hrs, with stirring. The mixture was filtered and the filtrate was evaporated to an oil. The oil was stirred with 100 ml of water for five mins and then extracted with ether. The ether extract was washed with water (2×), saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. After filtering, the solution was converted to 4.0 g (70%) of product, by treatment with ethereal oxalic acid. Recrystallization twice from ethyl acetate/methanol/ether yielded the analytical sample mp 188°-190° C. (dec).

Quelle