反応 #93153

反応方程式

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

N-(α,α,α-trifluoro-m-tolyl)piperazine

potassium carbonate

potassium iodide

→

product

収率 35.8%

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

収率 35.8%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度The reaction mixture was cooled
2. 2
   ろ過filtered
3. 3
   濃縮concentrated to an oil, which
4. 4
   抽出extracted with ether-ethyl acetate
5. 5
   洗浄The organic extracts were washed with water (2×), saturated sodium chloride solution
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   ろ過The mixture was filtered
8. 8
   濃縮concentrated to an oil, which
9. 9
   その他The salt was recrystallized from ethyl acetate/methanol

実験手順

A mixture of 6.5 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 5.8 g of N-(α,α,α-trifluoro-m-tolyl)piperazine, 7.0 g of potassium carbonate and a few crystals potassium iodide in 80 ml of dimethylformamide was stirred at 70°-75° C. for seven hrs. The reaction mixture was cooled, filtered and concentrated to an oil, which was stirred with water and extracted with ether-ethyl acetate. The organic extracts were washed with water (2×), saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The mixture was filtered and concentrated to an oil, which was converted to a salt by treatment with ethereal hydrogen chloride. The salt was recrystallized from ethyl acetate/methanol to give 4 g (35%) of product mp, 208°-209° C.

出典