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Oxalyl chloride → 4-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)benzoyl chloride

HRID 1196425
ノート
印刷プレビュー

反応式

HRID 1196425 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:14](=[O:15])[CH:13]=[CH:12][C:11]2=[O:16])=[CH:6][CH:5]=1)(O)=[O:2].C(Cl)(=O)C([Cl:20])=O>C1C=CC=CC=1>[C:14]1(=[O:15])[N:10]([C:7]2[CH:8]=[CH:9][C:4]([C:1]([Cl:20])=[O:2])=[CH:5][CH:6]=2)[C:11](=[O:16])[CH:12]=[CH:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 869254-(2,5-dihydro-2,5-dioxo-1H-pyrrol-1-yl)benzoic acid

生成物 1

HCID 133654044-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)benzoyl chloride

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Para-maleimidobenzoyl chloride was prepared in accordance with the procedure described by Adams et al. in J. Am. Chem. Soc., 42, 599 (1920). The N-(para-carboxyphenyl) maleimide (15 g) was suspended in about 80 ml of benzene with stirring. To this mixture was added 15 ml (a 2.5:1 molar excess) of oxalyl chloride, whereupon some gas was evolved. The mixture was then heated slowly to reflux and maintained at reflux for two hours. Excess oxalyl chloride was removed by distillation. The reaction mixture was then cooled and the yellow product recovered by suction filtration. The resultant product was washed with hexane and dried under vacuum at room temperature.

後処理

  1. additionTo this mixture was added 15 ml (a 2.5
  2. temperatureThe mixture was then heated slowly
  3. temperatureto reflux
  4. temperaturemaintained
  5. temperatureat reflux for two hours
  6. customExcess oxalyl chloride was removed by distillation
  7. temperatureThe reaction mixture was then cooled
  8. filtrationthe yellow product recovered by suction filtration
  9. washThe resultant product was washed with hexane
  10. customdried under vacuum at room temperature

出典と根拠

ORDレコード
ord-7c4bf3296ef7466abab096e780cf337d
出典データセット
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05114612

反応ノート

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