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Hydrochloric Acid → (2S)-2-(4-Bromophenyl)piperazine

HRID 1091376
Notes
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Reaction equation

HRID 1091376 reaction equation
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([C@H:9]2[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11][N:10]2C(OC(C)(C)C)=O)=[CH:5][CH:4]=1>C(OCC)(=O)C.CO>[Br:2][C:3]1[CH:4]=[CH:5][C:6]([C@H:9]2[CH2:14][NH:13][CH2:12][CH2:11][NH:10]2)=[CH:7][CH:8]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 53628944(S)-2-(4-bromophenyl)-1,4-di(t-butoxycarbonyl)piperazine

Product 1

HCID 51894714(2S)-2-(4-Bromophenyl)piperazine

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

Hydrogen chloride in ethyl acetate solution (4N) was added to a solution of di-tert-butyl (2S)-2-(4-bromophenyl)piperazine-1,4-dicarboxylate (10 g, 22.7 mmol) in methanol (50 ml). The mixture was stirred for one hour at room temperature and the solvent was evaporated under reduced pressure to give white solid. The mixture was partitioned between saturated aqueous sodium bicarbonate and chloroform. The organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo to afford (2S)-2-(4-bromophenyl)piperazine as white crystals. Benzylbromide (9.7 g, 56.7 mmol) was added to a solution of sodium hydride (60% in oil, 2.0 g, 50 mmol) and (2S)-2-(4-bromophenyl)piperazine in tetrahydrofuran (50 ml) at room temperature and the mixture was stirred for one hour. The mixture was partitioned between water and chloroform. The organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting 5-10% methanol in chloroform to furnish (2S)-1,4-Dibenzyl-2-(4-bromophenyl)piperazine (6.1 g, 64%) as a colorless oil.

Workup

  1. customthe solvent was evaporated under reduced pressure
  2. customto give white solid
  3. customThe mixture was partitioned between saturated aqueous sodium bicarbonate and chloroform
  4. washThe organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-a4db586f836d4f49bd3164542b156bec
Source dataset
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08129377B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes