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Pyridine → 2-(2-BROMO-5-METHOXYPHENYL)ETHANOL

HRID 1978896
Notes
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Reaction equation

HRID 1978896 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[CH2:6][CH2:7][OH:8].N1C=CC=CC=1.[Br:18]Br>ClCCl>[Br:18][C:9]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[CH2:6][CH2:7][OH:8]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 1049PyridineHCID 24408BromineHCID 787243-Methoxyphenethyl alcohol

Product 1

HCID 104896782-(2-BROMO-5-METHOXYPHENYL)ETHANOLYield 83.2%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a stirred mixture of 3-methoxyphenethyl alcohol (1.18 g, 7.8 mmol) and pyridine (0.75 ml, 9.3 mmol) in dry dichloromethane (10 ml) was added bromine (0.47 ml, 18.0 mmol) dropwise under nitrogen at 0° C. The orange solution was stirred at room temperature for 4 hours (hr). The reaction mixture was quenched by the addition of 10% sodium bisulfite aqueous solution., and extracted with dichloromethane. The organic extracts were washed with brine, dried over magnesium sulfate, and concentrated to give crude products, which were purified by silica-gel column chromatography eluted with gradient of hexane and ethyl acetate (10:1, 8:1, 5:1) to give the title compound as a colorless oil (1.5 g, 83.2%). 1H-NMR (CDCl3): 7.43 (d, J=8.8 Hz, 1H), 6.83 (d, J=3.3 Hz, 1H), 6.67 (dd, J=8,8, 3.3 Hz, 1H), 3.91-3.81 (m, 2H), 3.78 (s, 3H), 2.99 (t, J=6.6 Hz, 2H).

Workup

  1. customThe reaction mixture was quenched by the addition of 10% sodium bisulfite aqueous solution
  2. extraction, and extracted with dichloromethane
  3. washThe organic extracts were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customto give crude products, which
  7. customwere purified by silica-gel column chromatography
  8. washeluted with gradient of hexane and ethyl acetate (10:1, 8:1, 5:1)

Sources & evidence

ORD record
ord-7b04892886ad4946b33bf4feef0143fa
Source dataset
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06239147B1

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes