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Potassium Carbonate → HCID 86752938、化合物

HRID 1957532
ノート
印刷プレビュー

反応式

HRID 1957532 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([C:10](=[N:12][OH:13])[CH3:11])=[N:2]1.Br[CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22](=[CH:27][O:28][CH3:29])[C:23]([O:25][CH3:26])=[O:24].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([C:10](=[N:12][O:13][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22](=[CH:27][O:28][CH3:29])[C:23]([O:25][CH3:26])=[O:24])[CH3:11])=[N:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 53395349Methyl 2-[2-(bromomethyl)phenyl]-3-methoxyprop-2-enoateHCID 136351318HCID 136351318、化合物

生成物 1

HCID 86752938HCID 86752938、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 0.8 g of 1-(1,2-benzisoxazol-3-yl)ethanone oxime, 1.3 g of methyl 2-(bromomethyl)-α-(methoxymethylene)phenylacetate and 1 g of potassium carbonate in 15 ml of acetonitrile is refluxed for 4 h. The reaction mixture is cooled and filtered and the filtrate is concentrated under vacuum. The residue is dissolved in ethyl acetate and the solution is washed twice with water and once with a saturated solution of sodium chloride and dried over sodium sulfate. After removal of the solvent under vacuum, the residue is purified by chromatography on silica gel with ethyl acetate/hexane (1:3), giving the title compound having a melting point of 97°-98° C.

後処理

  1. temperatureis refluxed for 4 h
  2. temperatureThe reaction mixture is cooled
  3. filtrationfiltered
  4. concentrationthe filtrate is concentrated under vacuum
  5. dissolutionThe residue is dissolved in ethyl acetate
  6. washthe solution is washed twice with water and once with a saturated solution of sodium chloride
  7. dry with materialdried over sodium sulfate
  8. customAfter removal of the solvent under vacuum
  9. customthe residue is purified by chromatography on silica gel with ethyl acetate/hexane (1:3)

出典と根拠

ORDレコード
ord-0cc99ea2e0a44b829a9e6f5b3df9c44c
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05786374

反応ノート

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