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Ethanol → 5-(Trifluoromethyl)pyridin-2-ylamidoxime

HRID 1648419
ノート
印刷プレビュー

反応式

HRID 1648419 の反応式
C(O)C.[C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][N:7]=1)#[N:5].Cl.[NH2:17][OH:18].[OH-].[Na+]>ClCCCl.O>[F:14][C:12]([F:15])([F:13])[C:9]1[CH:10]=[CH:11][C:6]([C:4](=[N:17][OH:18])[NH2:5])=[N:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 15353725-(Trifluoromethyl)pyridine-2-carbonitrile

生成物 1

HCID 27793275-(Trifluoromethyl)pyridin-2-ylamidoxime収率 95.3%

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane
溶媒
HCID 962Water溶媒2 回

実験手順

180 ml of ethanol were added to a solution of 22 g of 2-cyano-5-trifluoromethylpyridine in 180 ml of 1,2-dichloroethane under stirring at room temperature, followed by drop-wise addition thereto of a solution of 9.8 g of hydroxylamine hydrochloride in 17 ml of water. An aqueous solution of 5.6 g of sodium hydroxide in 17 ml of water was drop-wise added to the resulting mixture. After completion of the drop-wise addition, the reaction mixture was heated at 80° C. for 2 hours. The reaction mixture was cooled, and stripped of insolubles by filtration. The filtrate was subjected to distillation under reduced pressure to remove therefrom the solvent. The resulting residue was washed with hexane. The precipitated solid was filtered off to obtain 25 g of 5-trifluoromethyl-2-pyridinecarboxamide oxime having a melting point of 130° to 133° C.

後処理

  1. additionfollowed by drop-wise addition
  2. additionAfter completion of the drop-wise addition
  3. temperaturethe reaction mixture was heated at 80° C. for 2 hours
  4. temperatureThe reaction mixture was cooled
  5. filtrationstripped of insolubles by filtration
  6. distillationThe filtrate was subjected to distillation under reduced pressure
  7. customto remove
  8. washThe resulting residue was washed with hexane
  9. filtrationThe precipitated solid was filtered off

出典と根拠

ORDレコード
ord-54a974a1ebab475bbd9862b7a6f3d909
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05436267

反応ノート

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