Bromine → 4-Bromo-2,3-difluoroaniline

HRID 81458

반응식

HRID 81458 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[NH2:9].[Br:10]Br>C(O)(=O)C>[Br:10][C:6]1[CH:5]=[CH:4][C:3]([NH2:9])=[C:2]([F:1])[C:7]=1[F:8]

참가 물질

4

반응물 2

HCID 24408BromineHCID 782782,3-Difluoroaniline

생성물 1

HCID 146210374-Bromo-2,3-difluoroaniline수율 30%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

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온도
0 °C

실험 절차

2,3-difluoro-phenylamine (13.45 g, 104.2 mmol) was diluted with acetic acid (180 ml), bromine (2.6 ml) diluted with acetic acid (5 ml) was slowly added thereto at 0° C., and the solution was stirred for 5 hours. The resulting solution was distilled under a reduced pressure to remove the solvent, basified by adding 50% sodium hydroxide solution (250 ml), and extracted with dichloromethane (200 ml) twice. The separated organic layer was dried over magnesium sulfate, filtered and distilled under a reduced pressure to obtain the title compound 6.46 g (yield: 30%).

후처리

  1. additionwas slowly added
  2. distillationThe resulting solution was distilled under a reduced pressure
  3. customto remove the solvent
  4. additionby adding 50% sodium hydroxide solution (250 ml)
  5. extractionextracted with dichloromethane (200 ml) twice
  6. dry with materialThe separated organic layer was dried over magnesium sulfate
  7. filtrationfiltered
  8. distillationdistilled under a reduced pressure

출처 및 근거

ORD 기록
ord-d65d2911c30a4fca89e708266d8929ec
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846699B2

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