HCID 22342622, compound → HCID 22342760, compound

HRID 584248Notes

Reaction equation

HRID 584248 reaction equation
[BrH:1].Br.C[O:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][C:17]=1[CH3:18])[CH2:8][CH:9]1[CH2:14][NH:13][CH2:12][CH2:11][NH:10]1>Br>[BrH:1].[BrH:1].[OH:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][C:17]=1[CH3:18])[CH2:8][CH:9]1[CH2:14][NH:13][CH2:12][CH2:11][NH:10]1

Participants

3

Reactant 1

HCID 22342622HCID 22342622, compound

Product 1

HCID 22342760HCID 22342760, compoundYield 151.4%

Reagents, catalysts & solvents 1

HCID 260Hydrogen BromideSolvent

Procedure

A stirred solution of 2-(3-methoxy-4-methylbenzyl)piperazine dihydrobromide (240 mg) in 48% hydrobromic acid (8 ml) was heated under reflux for 48 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was triturated with ethyl acetate and the resulting precipitates were collected by filtration, and washed with ethyl acetate to give 2-(3-hydroxy-4-methylbenzyl)piperazine dihydrobromide (175 mg) as a powder.

Workup

  1. temperatureunder reflux for 48 hours
  2. temperatureAfter cooling
  3. concentrationthe mixture was concentrated under reduced pressure
  4. customThe residue was triturated with ethyl acetate
  5. customthe resulting precipitates
  6. filtrationwere collected by filtration
  7. washwashed with ethyl acetate

Sources & evidence

ORD record
ord-d72d1313f2354b21b539e61ff0b912d1
Source dataset
uspto-grants-2005_08
Patent number
US06924278B2

Reaction notes

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