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Water → HCID 53956374、化合物

HRID 1288708
ノート
印刷プレビュー

反応式

HRID 1288708 の反応式
[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]
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 5

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

生成物 1

HCID 53956374HCID 53956374、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d655045780b641e8965d4b5be9d9456c
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05747424

反応ノート

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