反応 #93155

反応方程式

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

4-(4-methoxyphenyl)piperazine dihydrochloride

potassium carbonate

→

product

収率 86.6%

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

収率 86.6%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度cooled
2. 2
   ろ過filtered
3. 3
   その他the filtrate evaporated to an oil
4. 4
   workup.STIRRINGThe oil was stirred with 100 ml of water
5. 5
   抽出extracted with ether
6. 6
   抽出The ether extract
7. 7
   洗浄was washed with water (2×), saturated sodium chloride solution
8. 8
   乾燥dried over anhydrous magnesium sulfate
9. 9
   ろ過After filtering
10. 10
    workup.ADDITIONethereal oxalic acid was added
11. 11
    その他The precipitate was collected
12. 12
    その他dried

実験手順

To 40 ml of dimethylformamide was added 4.3 g 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 4.0 g of 4-(4-methoxyphenyl)piperazine dihydrochloride, 10.0 g of milled potassium carbonate, and 0.01 g potassium iodide. The mixture was stirred at 90° C. for two hrs, cooled, filtered, and the filtrate evaporated to an oil. The oil was stirred with 100 ml of water and extracted with ether. The ether extract was washed with water (2×), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, ethereal oxalic acid was added. The precipitate was collected and dried to yield 3.0 g (44%) of product. Two recrystallizations from ethyl acetate/methanol/ether (10:1:5) gave the analytical sample, mp 188°-189° C. (dec).

出典