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Water → HCID 53956374, 화합물

HRID 342966
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HRID 342966 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[CH:7]=[CH:6][C:5]=1[CH3:17])([O-:3])=[O:2].N1C=CC=CC=1.[OH-:24].[Na+].[Mn]([O-])(=O)(=O)=O.[K+].[OH2:32]>>[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:15])([F:16])[C:11]([F:12])([F:13])[F:14])[CH:7]=[CH:6][C:5]=1[C:17]([OH:32])=[O:24])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 962WaterHCID 1049PyridineHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 542079941-Methyl-2-nitro-4-(pentafluoroethyl)benzene

생성물 1

HCID 53956374HCID 53956374, 화합물

실험 절차

2-Nitro-4-pentafluoroethyltoluene (56.6 g) and pyridine (170 ml) were added to a stirred solution of sodium hydroxide (10.0 g) in water (500 ml). The mixture was stirred and heated at reflux and potassium permanganate (174 g) was added portionwise. The mixture was stirred and heated at reflux for 1 hour until the purple colouration had disappeared. After cooling, the mixture was filtered and the solid was washed with water (3×100 ml) and ether (300 ml). The layers were separated and the aqueous layer was washed with ether and acidified to pH 1. It was extracted with ether (3×300 ml) and the combined extracts were washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness to give 2-nitro-4-pentafluoroethylbenzoic acid (51.6 g) as a white solid mp 124°-135° C.

후처리

  1. temperatureheated
  2. temperatureat reflux
  3. stirringThe mixture was stirred
  4. temperatureheated
  5. temperatureat reflux for 1 hour until the purple colouration
  6. temperatureAfter cooling
  7. filtrationthe mixture was filtered
  8. washthe solid was washed with water (3×100 ml) and ether (300 ml)
  9. customThe layers were separated
  10. washthe aqueous layer was washed with ether
  11. extractionIt was extracted with ether (3×300 ml)
  12. washthe combined extracts were washed with water
  13. dry with materialdried (anhydrous magnesium sulphate)
  14. filtrationfiltered
  15. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-76dee83fa318471cb632451d4dca8aa6
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859283

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