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Water → HCID 76313010、化合物

HRID 266422
ノート
印刷プレビュー

反応式

HRID 266422 の反応式
[OH:1]/[N:2]=[C:3](\[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[O:14][C:15]1[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=1)/[C:4]([NH:6][CH3:7])=[O:5].[C:22](=O)([O-])[O-].[K+].[K+].COS(OC)(=O)=O.O>CC(C)=O>[CH3:22][O:1]/[N:2]=[C:3](\[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[O:14][C:15]1[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=1)/[C:4]([NH:6][CH3:7])=[O:5]
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 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 9795805HCID 9795805、化合物

生成物 1

HCID 76313010HCID 76313010、化合物収率 92.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

E-2-hydroxyimino-N-methyl-2-[2-(4-methylphenoxy) phenyl]acetoamide (1.00 g, 0.0035 mole) was dissolved in dried acetone (7 ml), and potassium carbonate (0.63 g, 0.0046 mole) and dimethylsulfate (0.53 g, 0.0042 mole) were added to the mixture, which was reacted at room temperature for 22 hours. After completion of the reaction, water was added to the reaction mixture, which was extracted twice with methylene chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain E-2-methoxyimino-N-methyl-2-[2-(4-methylphenoxy)phenyl]-acetamide as colorless crystals (0.96 g, yield: 92.3%).

後処理

  1. customwas reacted at room temperature for 22 hours
  2. additionwas added to the reaction mixture, which
  3. extractionwas extracted twice with methylene chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-6b8a34c223a9419eb5d079c1bf81aea5
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05650539

反応ノート

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