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Ethanethiol → HCID 178477296、化合物

HRID 1633423
ノート
印刷プレビュー

反応式

HRID 1633423 の反応式
[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([N+]([O-])=O)[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7].[CH2:20]([SH:22])[CH3:21].C([O-])(=O)C.[Na+]>C(OCC)(=O)C>[CH3:1][N:2]=[C:3]([OH:19])[C:4]1[C:5](=[C:9]([S:22][CH2:20][CH3:21])[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1)[C:6]([OH:8])=[O:7]
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 6343EthanethiolHCID 517045Sodium AcetateHCID 178485491HCID 178485491、化合物

生成物 1

HCID 178477296HCID 178477296、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

5.02 g (20 mmols) of 3,5-dinitrophthalic acid N-methylimide, 2.73 g (44 mmols) of ethylmercaptan, 8.2 g (1 0 mmols) of anhydrous sodium acetate and 50 ml of ethyl acetate are kept at 25° C. overnight and then kept under reflux, again overnight. The reaction mixture is evaporated, the residue is taken up in methylene chloride/water, the extracts are washed with saturated NaHCO3 solution, dried over sodium sulfate and evaporated and the residue is chromatographed with methylene chloride over 20 g of silica gel. After recrystallisation from methylene chloride/n-pentane, 2.40 g (45% of theory) of 3-ethylthio-5-nitrophthalic acid N-methylimide, with a melting point of 193°-4° C., are obtained.

後処理

  1. temperatureunder reflux, again overnight
  2. customThe reaction mixture is evaporated
  3. washthe extracts are washed with saturated NaHCO3 solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customthe residue is chromatographed with methylene chloride over 20 g of silica gel
  7. customAfter recrystallisation from methylene chloride/n-pentane, 2.40 g (45% of theory) of 3-ethylthio-5-nitrophthalic acid N-methylimide
  8. customwith a melting point of 193°-4° C., are obtained

出典と根拠

ORDレコード
ord-55661acaf59b4bdd914b876877a43d07
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04480105

反応ノート

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