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Water → 4-(Bromomethyl)-3,5-difluoropyridine

HRID 630010
Notes
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Reaction equation

HRID 630010 reaction equation
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([F:10])[C:7]=1[CH2:8]O.P(Br)(Br)[Br:12].O>C(Cl)(Cl)Cl>[Br:12][CH2:8][C:7]1[C:2]([F:1])=[CH:3][N:4]=[CH:5][C:6]=1[F:10]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 66815317(3,5-Difluoropyridin-4-yl)methanol

Product 1

HCID 668150974-(Bromomethyl)-3,5-difluoropyridineYield 83%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent2×

Procedure

To a solution of (3,5-difluoropyridin-4-yl)methanol (3.5 mmol) in anhydrous chloroform (15 mL) was added dropwise a solution of phosphorus tribromide (330 μL, 3.5 mmol) in anhydrous chloroform (5 mL) at 0° C. The mixture was stirred for 6 hours at room temperature. Water was added, and the reaction was extracted 3 times with dichloromethane. The combined organic phases were washed with brine and dried over magnesium sulfate. After evaporation of the solvent, 4-(bromomethyl)-3,5-difluoropyridine was obtained as pale yellow solid (600 mg, 83% yield for 2 steps) and used in the next step without purification; 1H NMR (400 MHz, MeOd4): δ 4.59 (s, 2H), 8.42 (s, 2H).

Workup

  1. extractionthe reaction was extracted 3 times with dichloromethane
  2. washThe combined organic phases were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customAfter evaporation of the solvent

Sources & evidence

ORD record
ord-5e11c569da604cbaa5a8610e35ce6feb
Source dataset
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09315521B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes