反応 #2271682

反応方程式

6-fluoro-3-(4-piperdinyl)-1,2-benzisoxazole

K2CO3

3-chloropropoxybenzene

acetonitrile

→

6-fluoro-3-[1-(3-phenoxypropyl)-4-piperidinyl)-1,2-benzisoxazole

収率 47.0%

溶媒

water

反応条件

後処理

1. 1
   温度at reflux under nitrogen for 30 hours
2. 2
   抽出the aqueous mixture was extracted with ethyl acetate
3. 3
   抽出The ethyl acetate extract
4. 4
   洗浄was washed with brine
5. 5
   その他dried with MgS04
6. 6
   濃縮concentrated
7. 7
   その他to afford 6.2 g of a damp, beige solid
8. 8
   その他The compound was recrystallized twice from ethanol

実験手順

A mixture of 6-fluoro-3-(4-piperdinyl)-1,2-benzisoxazole (4.0 g, 18.2 mmol). K2CO3 (3.0 g, 21.8 mmol), Kl (100 mg), 3-chloropropoxybenzene (3.4 g, 20.0 mmol), and acetonitrile was stirred at reflux under nitrogen for 30 hours. The reaction was poured into water and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate extract was washed with brine, dried with MgS04 and concentrated to afford 6.2 g of a damp, beige solid. The compound was recrystallized twice from ethanol to yield (47%) of 6-fluoro-3-[1-(3-phenoxypropyl)-4-piperidinyl)-1,2-benzisoxazole as a light beige solid, m.p.=78°-80° C.

出典