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Potassium Carbonate → HCID 10453356, 화합물

HRID 1792653
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HRID 1792653 반응식
[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:24][CH2:25][CH2:26][O:27][C:28]1[CH:33]=[CH:32][C:31]([C:34](=[O:36])[CH3:35])=[CH:30][CH:29]=1>C(#N)C>[F:1][C:2]1[CH:16]=[CH:15][C:5]2[C:6]([CH:9]3[CH2:10][CH2:11][N:12]([CH2:24][CH2:25][CH2:26][O:27][C:28]4[CH:33]=[CH:32][C:31]([C:34](=[O:36])[CH3:35])=[CH:30][CH:29]=4)[CH2:13][CH2:14]3)=[N:7][O:8][C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 8494213-(4-Piperidyl)-6-fluoro-1,2-benzisoxazoleHCID 10061000HCID 10061000, 화합물

생성물 1

HCID 10453356HCID 10453356, 화합물수율 48%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.27 g, 14.8 mmoles), K2CO3(3 g), 1-[4-(3-bromopropoxy)phenyl]ethanone (4.5 g, 17.5 mmoles) in acetonitrile (60 ml) was heated at reflux for 4 hr. The solvent was removed. The residue was dissolved in dichloromethane (300 ml) and washed with water and brine, then dried over MgSO4. The crude product from the evaporated solution was purified by flash chromatography (SiO2. 60 g; eluted with 1% methanol in dichloromethane, methane 1liter). The purest fractions were combined and gave 2.8 g, 48% of 1-[4-[3-[4-(6-fluoro-1,2benzisoxazol-3-yl)-1-piperidinyl]propoxy)phenyl]ethanone, m.p.=111°-112° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 4 hr
  3. customThe solvent was removed
  4. dissolutionThe residue was dissolved in dichloromethane (300 ml)
  5. washwashed with water and brine
  6. dry with materialdried over MgSO4
  7. customThe crude product from the evaporated solution was purified by flash chromatography (SiO2. 60 g; eluted with 1% methanol in dichloromethane, methane 1liter)

출처 및 근거

ORD 기록
ord-1a145ba0c2bc4bd290e7eaba5b81f228
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE039198E1

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