Dibenzofuran → 2-Bromodibenzofuran

HRID 1774279

반응식

HRID 1774279 반응식
[CH:1]1[C:9]2[C:8]3[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=3[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[Br:14]Br>C(O)(=O)C>[Br:14][C:2]1[CH:3]=[CH:4][C:5]2[O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=3[C:9]=2[CH:1]=1

참가 물질

4

반응물 2

HCID 568DibenzofuranHCID 24408Bromine

생성물 1

HCID 68562-Bromodibenzofuran

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Under a nitrogen atmosphere, 150 g of dibenzofuran and 1 l of acetic acid were loaded into a 300-ml three-necked flask, and then the contents were dissolved under heat. 188 Grams of bromine were added dropwise to the solution. After that, the mixture was stirred for 20 hours under air cooling. The precipitated crystal was separated by filtration, and was then sequentially washed with acetic acid and water. The washed crystal was dried under reduced pressure. The resultant crystal was purified by distillation under reduced pressure, and was then repeatedly recrystallized with methanol several times. Thus, 66.8 g of 2-bromodibenzofuran were obtained.

후처리

  1. dissolutionthe contents were dissolved
  2. temperatureunder heat
  3. temperaturecooling
  4. customThe precipitated crystal was separated by filtration
  5. washwas then sequentially washed with acetic acid and water
  6. customThe washed crystal was dried under reduced pressure
  7. distillationThe resultant crystal was purified by distillation under reduced pressure
  8. customwas then repeatedly recrystallized with methanol several times

출처 및 근거

ORD 기록
ord-82c3952324ca4f9ebf1ef9b6beeeffb6
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09260390B2

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