반응 #2271682

ord-b83a9d17e049439ba6fc72ccb4cde33e

반응 방정식

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
수율 47.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux under nitrogen for 30 hours
  2. 2
    추출the aqueous mixture was extracted with ethyl acetate
  3. 3
    추출The ethyl acetate extract
  4. 4
    세척was washed with brine
  5. 5
    기타dried with MgS04
  6. 6
    농축concentrated
  7. 7
    기타to afford 6.2 g of a damp, beige solid
  8. 8
    기타The compound was recrystallized twice from ethanol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE037729E1uspto-grants-2002_06