Potassium Carbonate → HCID 54340306、化合物

HRID 618725ノート

反応式

HRID 618725 の反応式
[F:1][C:2]1[C:3]([F:13])=[CH:4][C:5]2[O:9][C:8]([C:10]#[N:11])=[CH:7][C:6]=2[CH:12]=1.Cl.[NH2:15][OH:16].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:1][C:2]1[C:3]([F:13])=[CH:4][C:5]2[O:9][C:8]([C:10](=[N:15][OH:16])[NH2:11])=[CH:7][C:6]=2[CH:12]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 218483295,6-Difluoro-2-benzofurancarbonitrile

生成物 1

HCID 54340306HCID 54340306、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1.2 g (6.7 mmol) of 5,6-difluorobenzofuran-2-carbonitrile, 0.93 g (13.4 mmol) of hydroxylamine hydrochloride, 2.78 g (20.1 mmol) of potassium carbonate and 50 ml of anhydrous ethanol was heated under reflux over 16 hours while stirring. Subsequently, the solid was filtered off and the filtrate was concentrated in a vacuum. The crude product obtained was purified by column chromatography on silica gel (ethyl acetate/hexane 3:2). There was obtained 0.88 g (61%) of 5,6-difluorobenzofuran-2-carboxamidoxime as a light yellow solid with m.p. 184°.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux over 16 hours
  3. filtrationSubsequently, the solid was filtered off
  4. concentrationthe filtrate was concentrated in a vacuum
  5. customThe crude product obtained
  6. customwas purified by column chromatography on silica gel (ethyl acetate/hexane 3:2)

出典と根拠

ORDレコード
ord-d2823137acf746baa079c71190e3f402
出典データセット
uspto-grants-1999_09
特許番号
US05955495

反応ノート

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