反应 #2271682

ord-b83a9d17e049439ba6fc72ccb4cde33e

反应方程式

Fc1ccc2c(C3CCNCC3)noc2c1
6-fluoro-3-(4-piperdinyl)-1,2-benzisoxazole
O=C([O-])[O-].[K+].[K+]
K2CO3
ClCCCOc1ccccc1
3-chloropropoxybenzene
CC#N
acetonitrile
Fc1ccc2c(C3CCN(CCCOc4ccccc4)CC3)noc2c1
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. 1
    温度at reflux under nitrogen for 30 hours
  2. 2
    萃取the aqueous mixture was extracted with ethyl acetate
  3. 3
    萃取The ethyl acetate extract
  4. 4
    洗涤was washed with brine
  5. 5
    其他dried with MgS04
  6. 6
    浓缩concentrated
  7. 7
    其他to afford 6.2 g of a damp, beige solid
  8. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE037729E1uspto-grants-2002_06