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Piperazine → HCID 67141098, compound

HRID 1864426
Notes
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Reaction equation

HRID 1864426 reaction equation
[Br:1][C:2]1[C:3](Cl)=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1.[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.C(N(CC)CC)C>C(#N)C>[Br:1][C:2]1[C:3]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 4837PiperazineHCID 8471TriethylamineHCID 27344183-Bromo-2-chloro-6-methylpyridine

Product 1

HCID 67141098HCID 67141098, compoundYield 20.3%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A solution of 3-bromo-2-chloro-6-picoline (0.2 g), piperazine (0.083 g) and triethylamine (0.096 g) in acetonitrile (5 ml) was heated in the microwave apparatus: 30 min at 120° C. followed by 60 min at 150° C. and 30 min at 170° C. The mixture was concentrated and the product was purified by chromatography (SiO2, CH2Cl2=>CH2Cl2/CH3OH 4:1) to give 1-(3-bromo-6-methyl-pyridin-2-yl)-piperazine (0.05 g) as a light yellow solid.

Workup

  1. concentrationThe mixture was concentrated
  2. customthe product was purified by chromatography (SiO2, CH2Cl2=>CH2Cl2/CH3OH 4:1)

Sources & evidence

ORD record
ord-23966f69fd7f4fbd94dde6e0ed513270
Source dataset
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07625902B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes