反应 #2271682
ord-b83a9d17e049439ba6fc72ccb4cde33e
反应方程式
6-fluoro-3-(4-piperdinyl)-1,2-benzisoxazole
K2CO3
3-chloropropoxybenzene
acetonitrile
→
6-fluoro-3-[1-(3-phenoxypropyl)-4-piperidinyl)-1,2-benzisoxazole
收率 47.0%
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度at reflux under nitrogen for 30 hours
- 2萃取the aqueous mixture was extracted with ethyl acetate
- 3萃取The ethyl acetate extract
- 4洗涤was washed with brine
- 5其他dried with MgS04
- 6浓缩concentrated
- 7其他to afford 6.2 g of a damp, beige solid
- 8其他The compound was recrystallized twice from ethanol
实验过程
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.