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

HRID 1761643노트

반응식

HRID 1761643 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-323cb1c41539483a969603e97957f6ad
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04826982

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