Acetic Acid → 2-Bromodibenzofuran

HRID 1048838

반응식

HRID 1048838 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.C(O)(=O)C.[Br:18]Br>O>[Br:18][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

5

반응물 3

HCID 176Acetic AcidHCID 568DibenzofuranHCID 24408Bromine

생성물 1

HCID 68562-Bromodibenzofuran수율 31%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

150 g of dibenzofuran (892 millimoles) and 1 liter of acetic acid were placed in a flask, which was then replaced with nitrogen and the contents of which were dissolved under heating. After 188 g of bromine (1.18 moles) were dropped while being occasionally cooled with water, the mixture was stirred for 20 hours under cooling with air. The precipitated crystals were filtrated, washed sequentially with acetic acid and water, and dried under reduced pressure. After the crystals obtained were purified by distillation under reduced pressure, recrystallization from methanol was performed several times to obtain 66.8 g of 2-bromodibenzofuran (yield 31%). The resultant was identified as Intermediate 4 by FD-MS analysis.

후처리

  1. dissolutionthe contents of which were dissolved
  2. temperatureunder heating
  3. temperatureunder cooling with air
  4. filtrationThe precipitated crystals were filtrated
  5. washwashed sequentially with acetic acid and water
  6. customdried under reduced pressure
  7. customAfter the crystals obtained
  8. distillationwere purified by distillation under reduced pressure, recrystallization from methanol

출처 및 근거

ORD 기록
ord-285b2d99a93a478ba3a119d70c072aa4
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382206B2

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