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Diethyl Ether → 7-Bromo-1-benzofuran

HRID 1254276
Notes
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Reaction equation

HRID 1254276 reaction equation
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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

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

Product 1

HCID 1136287-Bromo-1-benzofuranYield 38%

Reagents, catalysts & solvents 1

HCID 7964ChlorobenzeneSolvent2×

Procedure

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 1M 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.

Workup

  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

Sources & evidence

ORD record
ord-6a15ac69865240d8a047aec0e0c9957b
Source dataset
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08455521B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes