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Iodoethane → HCID 86740954、化合物

HRID 364627
ノート
印刷プレビュー

反応式

HRID 364627 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=[N:17][OH:18])[CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1.[H-].[Na+].[CH2:21](I)[CH3:22]>C(COC)OC>[CH2:21]([O:18][N:17]=[C:9]([C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1])[CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)[CH3:22]
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 6340IodoethaneHCID 24758Sodium hydrideHCID 71415949N-[1-(2,4-Dichlorophenyl)-2-(pyridin-3-yl)ethylidene]hydroxylamine

生成物 1

HCID 86740954HCID 86740954、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of 3 g of 2',4'-dichloro-2-(3-pyridyl)-acetophenone oxime in 25 ml of dimethoxyethane is treated portionwise with 0.51 g of sodium hydride dispersion (55% in oil) and the mixture is stirred for 30 minutes at room temperature. Thereupon, 2.0 g of ethyl iodide are added and the mixture is heated at reflux temperature. After 4 hours, the mixture is poured onto ice and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated under reduced pressure. The crude product is purified by chromatography on silica gel to yield 2',4'-dichloro-2-(3-pyridyl)-acetophenone O-ethyl oxime as a yellowish oil.

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux temperature
  3. waitAfter 4 hours
  4. additionthe mixture is poured onto ice
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic phase is dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe crude product is purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-0a49592123134bd585cd2ef112d1106d
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04605656

反応ノート

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