Bromine → HCID 87377841, compound

HRID 1843076Notes

Reaction equation

HRID 1843076 reaction equation
[Br:1]Br.[CH3:3][N:4]1[CH:8]=[CH:7][C:6]([C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])=[N:5]1>O>[Br:1][C:7]1[C:6]([C:9]([F:17])([F:18])[C:10]([F:15])([F:16])[C:11]([F:12])([F:13])[F:14])=[N:5][N:4]([CH3:3])[CH:8]=1

Participants

4

Reactant 2

HCID 24408BromineHCID 87377840HCID 87377840, compound

Product 1

HCID 87377841HCID 87377841, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

At 40° C., 3.27 g (20.5 mmol) of bromine are added dropwise to a solution of 4.65 g (18.6 mmol) of 1-methyl-3-heptafluoropropyl-1H-pyrazole in 18 ml of water and the reaction mixture is afterstirred firstly for one hour at 60° C. and then for 18 hours at room temperature. The aqueous phase is extracted three times with dichloromethane and the organic phase is dried over sodium sulphate. The dichloromethane is distilled off at reduced pressure on a rotary evaporator. This gives 5.75 g of 1-methyl-3-heptafluoropropyl-4-bromo-1H-pyrazole (78%) as an oil.

Workup

  1. waitfor 18 hours at room temperature
  2. extractionThe aqueous phase is extracted three times with dichloromethane
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. distillationThe dichloromethane is distilled off at reduced pressure on a rotary evaporator

Sources & evidence

ORD record
ord-079131de89604c7d86f73e01f34753be
Source dataset
uspto-grants-2015_02
Patent number
US08946234B2

Reaction notes

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