Bromine → 2-Bromo-3-chloro-4-fluoro-6-nitroaniline

HRID 1761643ノート

反応式

HRID 1761643 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:6]([N+:10]([O-:12])=[O:11])=[CH:7][C:8]=1[F:9])[NH2:5].[Br:13]Br>C(O)(=O)C>[Br:13][C:3]1[C:2]([Cl:1])=[C:8]([F:9])[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:4]=1[NH2:5]

参加物

4

反応物 2

HCID 24408BromineHCID 5178355-Chloro-4-fluoro-2-nitroaniline

生成物 1

HCID 137487952-Bromo-3-chloro-4-fluoro-6-nitroaniline

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Into a solution of 3-chloro-4-fluoro-6-nitroaniline (200.3 g) in acetic acid (1.5 litter) was added bromine (339 g) during a period of 80 minutes at 50° C. under stirring and stirred for further 2 hours. The reaction mixture was poured into ice water (3 litter) and the resulting precipitate was collected by filtration, washed with water and added to a mixture of concentrated hydrochloric acid (300 ml) and ethanol (1.2 litter). The mixture was refluxed for 8.5 hrs. After cooling, the precipitate was collected by filtration and washed with water and dried. The title compound thus obtained weighed 235.6 g as yellow needles, mp 146°-147° C.

後処理

  1. stirringstirred for further 2 hours
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. additionadded to a mixture of concentrated hydrochloric acid (300 ml) and ethanol (1.2 litter)
  5. temperatureThe mixture was refluxed for 8.5 hrs
  6. temperatureAfter cooling
  7. filtrationthe precipitate was collected by filtration
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-323cb1c41539483a969603e97957f6ad
出典データセット
uspto-grants-1989_05
特許番号
US04826982

反応ノート

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