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Potassium Carbonate → HCID 86752898、化合物

HRID 1955851
ノート
印刷プレビュー

反応式

HRID 1955851 の反応式
FC1C=CC2C(C3CCNCC3)=NOC=2C=1.C([O-])([O-])=O.[K+].[K+].BrCCCO[C:28]1[CH:33]=[CH:32][C:31]([C:34](=[O:36])[CH3:35])=[CH:30][CH:29]=1.[F:37][C:38]1[CH:65]=[CH:64][C:41]2[C:42]([CH:45]3[CH2:50][CH2:49][N:48]([CH2:51][CH2:52][CH2:53][O:54]C4C=CC(C(=O)C)=CC=4)[CH2:47][CH2:46]3)=[N:43][O:44][C:40]=2[CH:39]=1>C(#N)C>[F:37][C:38]1[CH:65]=[CH:64][C:41]2[C:42]([CH:45]3[CH2:50][CH2:49][N:48]([CH2:51][CH2:52][C:53]([C:28]4[CH:29]=[CH:30][C:31]([C:34](=[O:36])[CH3:35])=[CH:32][CH:33]=4)=[O:54])[CH2:47][CH2:46]3)=[N:43][O:44][C:40]=2[CH:39]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 8494213-(4-Piperidyl)-6-fluoro-1,2-benzisoxazoleHCID 10061000HCID 10061000、化合物HCID 10453356HCID 10453356、化合物

生成物 1

HCID 86752898HCID 86752898、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 6fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.27 & 14.8 mmol), K2CO3 (3 g), 1-[4-(3-bromopropoxy)phenyl]ethanone (4.5 g, 17.5 mmol) in acetonitrile (60 ml) was heated at reflux for 4 hours. 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, 1 liter). The purest fractions were combined and gave 2.8 g, 48%, of 1-[4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]phenyl]ethanone, m.p.=111-112° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  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, 1 liter)
  8. customgave 2.8 g, 48%

出典と根拠

ORDレコード
ord-66055026e93049dba65b1730faeda416
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05776963

反応ノート

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