Hydrochloric Acid → 4-Chloro-2-methyl-3-(trifluoromethyl)aniline

HRID 723707ノート

反応式

HRID 723707 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8]C(=O)C(C)(C)C)=[C:4]([CH3:15])[C:3]=1[C:16]([F:19])([F:18])[F:17].Cl>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([CH3:15])[C:3]=1[C:16]([F:17])([F:18])[F:19]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21874848N-[4-chloro-2-methyl-3-(trifluoromethyl)phenyl]-2,2-dimethylpropanamide

生成物 1

HCID 179957894-Chloro-2-methyl-3-(trifluoromethyl)aniline収率 76%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

N-(4-Chloro-2-methyl-3-trifluoromethylphenyl)-2,2-dimethyl-propionamide 1.0 g, 3.4 mmol) was added to a 1:1 mixture (15 mL) of concentrated HCl and ethanol and heated at reflux for overnight. The reaction was cooled and concentrated in vacuo to give a tan solid which was then partitioned between EtOAc and saturated NaHCO3. The organic layer was separated, washed with water, brine, dried (Na2SO4), filtered and concentrated to give compound 760C (0.54g, 76%) as a brown oily solid.

後処理

  1. temperatureheated
  2. temperatureat reflux for overnight
  3. temperatureThe reaction was cooled
  4. concentrationconcentrated in vacuo
  5. customto give a tan solid which
  6. customwas then partitioned between EtOAc and saturated NaHCO3
  7. customThe organic layer was separated
  8. washwashed with water, brine
  9. dry with materialdried (Na2SO4)
  10. filtrationfiltered
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-e79b05be6b1746ca8edb2186708f812d
出典データセット
uspto-grants-2006_11
特許番号
US07141578B2

反応ノート

読み込み中…