Phosphorus tribromide → HCID 68614005, compound

HRID 2189144Notes

Reaction equation

HRID 2189144 reaction equation
P(Br)(Br)[Br:2].[Br:5][C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([F:13])=[CH:8][C:7]=1[CH2:14]O>ClCCl.C(OCC)C>[Br:5][C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([F:13])=[CH:8][C:7]=1[CH2:14][Br:2]

Participants

5

Reactant 2

HCID 24614Phosphorus tribromideHCID 68615123HCID 68615123, compound

Product 1

HCID 68614005HCID 68614005, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 6344DichloromethaneSolvent

Procedure

0.55 mmol of phosphorous tribromid is added dropwise to a solution of 1 mmol of (2-Bromo-4-chloro-5-fluoro-phenyl)-methanol in 40 ml of dichloromethane. The trouble reaction solution is stirred at room temperature for 2 hours, diluted with 100 ml of diethylether and decanted. The supernatant is washed with 10 ml of 2N sodium bicarbonate solution, 20 ml of water and 20 ml of brine, dried over sodium sulfate, filtered and concentrated under reduced pressure at 28° C. to afford the title compound which is identified based on the Rf value.

Workup

  1. customThe trouble reaction solution
  2. customdecanted
  3. washThe supernatant is washed with 10 ml of 2N sodium bicarbonate solution, 20 ml of water and 20 ml of brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure at 28° C.

Sources & evidence

ORD record
ord-895d088489624661906578b3b338fe21
Source dataset
uspto-grants-2012_12
Patent number
US08324235B2

Reaction notes

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