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Phosphorus tribromide → 1-(Bromomethyl)-4-iodo-2-(trifluoromethyl)benzene

HRID 1946394
Notes
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Reaction equation

HRID 1946394 reaction equation
[I:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]O)=[C:4]([C:10]([F:13])([F:12])[F:11])[CH:3]=1.P(Br)(Br)[Br:15].C(=O)([O-])O.[Na+]>C(Cl)Cl>[Br:15][CH2:8][C:5]1[CH:6]=[CH:7][C:2]([I:1])=[CH:3][C:4]=1[C:10]([F:13])([F:12])[F:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 24614Phosphorus tribromideHCID 516892Sodium BicarbonateHCID 66770401(4-Iodo-2-(trifluoromethyl)phenyl)methanol

Product 1

HCID 667721121-(Bromomethyl)-4-iodo-2-(trifluoromethyl)benzeneYield 48.9%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent3×

Procedure

To a solution of [4-iodo-2-(trifluoromethyl)phenyl]methanol (2.1 g, 6.95 mmol) in DCM (15 ml) in an ice-water bath was added dropwise a solution of phosphorous tribromide (0.66 ml, 7.00 mmol, Aldrich) in DCM (15 ml). The resulting solution was allowed to warm to ambient temperature and stirred under nitrogen for 2 h. The reaction mixture was poured onto a mixture of ice-water (50 ml) and saturated sodium hydrogen carbonate (50 ml). The biphasic mixture was diluted with DCM (50 ml). The phases were separated and the aqeuous phase washed with DCM (50 ml). The combined organic phases were washed with water (50 ml), dried (MgSO4), filtered and the solvent removed in vacuo to leave 1-(bromomethyl)-4-iodo-2-(trifluoromethyl)benzene as a brown oil (1.24 g).

Workup

  1. customThe phases were separated
  2. washthe aqeuous phase washed with DCM (50 ml)
  3. washThe combined organic phases were washed with water (50 ml)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

Sources & evidence

ORD record
ord-58a1c34a813243bfa2fedf082244a046
Source dataset
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08399436B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes