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

HRID 1034332
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HRID 1034332 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4070919f56f64e2795aac29f46e169ad
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05315011

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