Phosphorus tribromide → HCID 22934897, compound
Reaction equation
[CH2:1]([N:3]1[C:7]([F:8])=[C:6]([CH2:9]O)[C:5]([C:11]([F:14])([F:13])[F:12])=[N:4]1)[CH3:2].P(Br)(Br)[Br:16]>C(OCC)C>[Br:16][CH2:9][C:6]1[C:5]([C:11]([F:14])([F:13])[F:12])=[N:4][N:3]([CH2:1][CH3:2])[C:7]=1[F:8]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- -10 °C
Procedure
A solution of 9.1 g (42.9 mmoles) of (1-ethyl-5-fluoro-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol dissolved in 100 ml of diethyl ether was cooled to −10° C. Thereto was added 12.2 g (45.0 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water and extraction with diethyl ether was conducted. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein, to obtain a crude product of 4-bromomethyl-1-ethyl-5-fluoro-3-trifluoromethyl-1H-pyrazole.
Workup
- customto give rise
- customto a reaction
- customAfter the completion of the reaction
- washThe resulting organic layer was washed with an aqueous sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe resulting solution was subjected to reduced pressure distillation
- customto remove the solvent
Sources & evidence
- ORD record
- ord-6005a5a792734264b6023372d5b7516b
- Source dataset
- uspto-grants-2011_01
- Patent number
- US07875606B2
Reaction notes
Loading…