Hydrochloric Acid → 2-Nitro-4-(trifluoromethyl)phenol

HRID 261188

反応式

HRID 261188 の反応式
[OH-:1].[Na+].[N+:3]([C:6]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[CH:8][C:7]=1Cl)([O-:5])=[O:4].O.Cl>CS(C)=O>[N+:3]([C:6]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[CH:8][C:7]=1[OH:1])([O-:5])=[O:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 14798Sodium Hydroxide

生成物 1

HCID 98162-Nitro-4-(trifluoromethyl)phenol

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

87.6 g of finely powdered sodium hydroxide was added in portions over an 8-hour period to a stirred solution of 165.0 g of 2-nitro-4-(trifluoromethyl)chlorobenzene in 220 ml of dimethyl sulfoxide at room temperature. The mixture was allowed to stand overnight, then poured into 1.5 liters of cold water. The resulting mixture was acidified to pH 1 with concentrated hydrochloric acid. An oil formed; it was separated and dissolved in ether. The solution was dried (MgSO4) and stripped of solvent under reduced pressure. The residue was mixed with cold sodium hydroxide solution and the mixture was extracted with petroleum ether. The water layer was acidified with concentrated hydrochloric acid. The resulting oil was separated and dissolved in ether. The solution was dried (MgSO4) and stripped of solvent to give 2-nitro-4-(trifluoromethyl)phenol (6A).

後処理

  1. customAn oil formed
  2. customit was separated
  3. dissolutiondissolved in ether
  4. dry with materialThe solution was dried (MgSO4)
  5. additionThe residue was mixed with cold sodium hydroxide solution
  6. extractionthe mixture was extracted with petroleum ether
  7. customThe resulting oil was separated
  8. dissolutiondissolved in ether
  9. dry with materialThe solution was dried (MgSO4)

出典と根拠

ORDレコード
ord-74c9b8f633a54154b305fbb2fe0d3f4c
出典データセット
uspto-grants-1979_08
特許番号
US04164576

関連ノート

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