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

HRID 2356007노트

반응식

HRID 2356007 반응식
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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 24014Cupric Chloride촉매HCID 6342Acetonitrile용매

반응 조건

온도
70 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-8bf5ece002124a2fbadcfde6e698e8d7
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754886B2

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