Hydrochloric Acid → 2-Methoxy-5-(trifluoromethyl)aniline

HRID 868399

反応式

HRID 868399 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N+:13]([O-])=O.Cl>C(O)(C)C.O.[Fe]>[NH2:13][C:4]1[CH:5]=[C:6]([C:9]([F:10])([F:11])[F:12])[CH:7]=[CH:8][C:3]=1[O:2][CH3:1]

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 967482-Nitro-4-trifluoromethylanisole

生成物 1

HCID 6006372-Methoxy-5-(trifluoromethyl)aniline収率 82.8%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 962Water溶媒HCID 3776Isopropanol溶媒

反応条件

温度
50 °C

実験手順

4-Methoxy-3-nitrobenzotrifluoride (95 g) in isopropanol (1.0 liter) and water (250 ml) was mixed with concentrated hydrochloric acid (15 ml). Iron powder (180 g) was added and the mixture was heated and stirred under reflux. After 90 minutes the mixture was cooled to 50° C. and filtered. The residue was washed with isopropanol and the combined filtrates evaporated. The residue was dissolved in toluene and the solution dried (MgSO4) and evaporated. The residue was triturated with light petroleum (b.p. 30°-40°) to give the 3-amino-4-methoxybenzotrifluoride as a colourless solid (68 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. washThe residue was washed with isopropanol
  5. customthe combined filtrates evaporated
  6. dissolutionThe residue was dissolved in toluene
  7. dry with materialthe solution dried (MgSO4)
  8. customevaporated
  9. customThe residue was triturated with light petroleum (b.p. 30°-40°)

出典と根拠

ORDレコード
ord-5eb17cae1abe4f1f8240e585bdc7150e
出典データセット
uspto-grants-1988_10
特許番号
US04778914

関連ノート

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