Hydrochloric Acid → 4-Bromo-1-chloro-2-(trifluoromethoxy)benzene

HRID 2356007ノート

反応式

HRID 2356007 の反応式
N(OC(C)(C)C)=O.[Br:8][C:9]1[CH:15]=[CH:14][C:12](N)=[C:11]([O:16][C:17]([F:20])([F:19])[F:18])[CH:10]=1.[ClH:21]>C(#N)C.[Cu](Cl)Cl>[Br:8][C:9]1[CH:15]=[CH:14][C:12]([Cl:21])=[C:11]([O:16][C:17]([F:20])([F:19])[F:18])[CH:10]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 10906Tert-Butyl nitriteHCID 7373824-Bromo-2-(trifluoromethoxy)aniline

生成物 1

HCID 227302024-Bromo-1-chloro-2-(trifluoromethoxy)benzene

試薬・触媒・溶媒 2

HCID 24014Cupric Chloride触媒HCID 6342Acetonitrile溶媒

反応条件

温度
70 °C

実験手順

A mixture of tert-butyl nitrite (1.78 mL, 15.0 mmol), copper (II) chloride (1.61 g, 12.0 mmol) and 4-bromo-2-(trifluoromethoxy)aniline (2.56 g, 10.0 mmol) in acetonitrile (40 mL) was heated to 70° C., stirred for 3 hours, cooled to room temperature, poured into 0.5M HCl, and extracted with diethyl ether. The combined extracts were washed with water and brine, dried (MgSO4), filtered, and concentrated to provide the desired product. MS (ESI(+)) m/e 275 (M+H)+.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with diethyl ether
  3. washThe combined extracts were washed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-8bf5ece002124a2fbadcfde6e698e8d7
出典データセット
uspto-grants-2010_07
特許番号
US07754886B2

反応ノート

読み込み中…