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

HRID 341738ノート

反応式

HRID 341738 の反応式
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

参加物

8

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 62652Cuprous chloride触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fdf4db2069834267a19313abb8d6b659
出典データセット
uspto-grants-1999_01
特許番号
US05856274

反応ノート

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