Hydrochloric Acid → 6-Bromo-3-chloro-2-fluorobenzotrifluoride

HRID 341738

반응식

HRID 341738 반응식
N([O-])=O.[Na+].[Br:5][C:6]1[CH:12]=[CH:11][C:9](N)=[C:8]([F:13])[C:7]=1[C:14]([F:17])([F:16])[F:15].[ClH:18]>S(=O)(=O)(O)O.C(O)(=O)C.O.[Cu]Cl>[Br:5][C:6]1[C:7]([C:14]([F:17])([F:16])[F:15])=[C:8]([F:13])[C:9]([Cl:18])=[CH:11][CH:12]=1

참가 물질

8

반응물 3

HCID 313Hydrochloric AcidHCID 23668193Sodium NitriteHCID 536697144-Bromo-2-fluoro-3-(trifluoromethyl)aniline

생성물 1

HCID 536324436-Bromo-3-chloro-2-fluorobenzotrifluoride

시약·촉매·용매 4

HCID 62652Cuprous chloride촉매HCID 176Acetic Acid용매HCID 962Water용매HCID 1118Sulfuric Acid용매

실험 절차

A solution of sodium nitrite (7.3 g) in concentrated sulphuric acid was added to a stirred cooled solution of 4-bromo-2-fluoro-3-trifluoromethylaniline (27.4 g) in glacial acetic acid while maintaining the temperature below 15° C. The mixture was stirred at 10°-15° C. for one and a half hours then poured into a mixture of copper (I) chloride (10.5 g) in hydrochloric acid (5M). The mixture was stirred for one and a half hours then diluted with water, extracted with ether, washed with aqueous sodium hydroxide solution (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 6-bromo-3-chloro-2-fluorobenzotrifluoride (8.3 g) as a yellow oil b.p. 44°-45° C./2 mbar.

후처리

  1. temperaturewhile maintaining the temperature below 15° C
  2. stirringThe mixture was stirred for one and a half hours
  3. extractionextracted with ether
  4. washwashed with aqueous sodium hydroxide solution (2M), water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness
  8. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-fdf4db2069834267a19313abb8d6b659
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856274

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