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Diethyl Ether → 7-Bromo-1-benzofuran

HRID 2355396
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HRID 2355396 반응식
C(O[CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[Br:13])C.[OH-].[Na+].CCOCC>ClC1C=CC=CC=1>[Br:13][C:8]1[C:7]2[O:6][CH:5]=[CH:4][C:12]=2[CH:11]=[CH:10][CH:9]=1
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참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 229514321-Bromo-2-(2,2-diethoxyethoxy)benzene

생성물 1

HCID 1136287-Bromo-1-benzofuran수율 38%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매2회

실험 절차

A stirred mixture of polyphosphoric acid (˜5 g) and chlorobenzene (8 mL) was heated at reflux and a solution of 1-(2,2-diethoxyethoxy)-2-bromobenzene (2.62 g, 9.0 mmol) in chlorobenzene (3 mL) was added dropwise over 10 min. The mixture was heated at reflux for 1.5 h. The mixture was allowed to cool to rt and 1 M aq NaOH (20 mL) was added, followed by ether (175 mL). The mixture was washed with water (2×20 mL) and brine (20 mL), and dried over MgSO4. Evaporation of the solvent left a residue which was purified by a chromatography on a 140-g silica cartridge eluted with hexanes and a 0-10% EtOAc in hexanes gradient. Appropriate fractions were pooled and concentrated to afford 7-bromobenzofuran (0.65 g, 38% from 2-bromophenol) as a clear colorless oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux
  3. temperatureThe mixture was heated
  4. temperatureat reflux for 1.5 h
  5. washThe mixture was washed with water (2×20 mL) and brine (20 mL)
  6. dry with materialdried over MgSO4
  7. customEvaporation of the solvent
  8. waitleft a residue which
  9. customwas purified by a chromatography on a 140-g silica cartridge
  10. washeluted with hexanes
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5448868ecc834b0187ad4ed1a6f54691
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754737B2

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