반응 #2271668

ord-5b33fe3929024bc59431748dcaa202b6

반응 방정식

Cl.Fc1ccc2c(C3CCNCC3)noc2c1
6-fluoro-3-(4-piperidinyl)-1,2 benzisoxazole hydrochloride
O=C([O-])[O-].[K+].[K+]
K2CO3
COc1cc(C(C)=O)ccc1OCCCCl
1-[4-(3-chloropropoxy)-3-methoxyphenyl]ethanone
CN(C)C=O
dimethylformamide
COc1cc(C(C)=O)ccc1OCCCN1CCC(c2noc3cc(F)ccc23)CC1
1-[4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3-methoxyphenyl]-ethanone
수율 58.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the aqueous mixture was extracted with ethyl acetate
  2. 2
    세척The ethyl acetate was washed (water)
  3. 3
    건조dried (MgSO4)
  4. 4
    농축concentrated
  5. 5
    기타to afford a moist solid
  6. 6
    기타Recrystallization (twice) from ethyl alcohol

실험 절차

A stirred mixture of 6-fluoro-3-(4-piperidinyl)-1,2 benzisoxazole hydrochloride (5.1 g, 20 mmol). K2CO3 (5.2 g, 40 mmol), 1-[4-(3-chloropropoxy)-3-methoxyphenyl]ethanone (5.3 g, 22 mmol), and dimethylformamide (60 ml) was heated at 90° C. for 16 hours. The reaction was poured into water, and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate was washed (water), dried (MgSO4) and concentrated to afford a moist solid. Recrystallization (twice) from ethyl alcohol afforded 5.0 g (58%) of 1-[4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3-methoxyphenyl]-ethanone as a beige solid, m.p.=118°-120° C.

출처

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