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Hydrochloric Acid → 1-(6-Bromonaphth-2-ylsulphonyl)piperazine hydrochloride

HRID 278552
Notes
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Reaction equation

HRID 278552 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:26]=[CH:25][C:24]3[C:19](=[CH:20][CH:21]=[C:22]([Br:27])[CH:23]=3)[CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.CO.[ClH:30]>C(OCC)(=O)C>[ClH:30].[Br:27][C:22]1[CH:23]=[C:24]2[C:19](=[CH:20][CH:21]=1)[CH:18]=[C:17]([S:14]([N:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)(=[O:15])=[O:16])[CH:26]=[CH:25]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 22628201Tert-butyl 4-[(6-bromo-2-naphthyl)sulfonyl]piperazinecarboxylate

Product 1

HCID 223297171-(6-Bromonaphth-2-ylsulphonyl)piperazine hydrochloride

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To the obtained 1-(tert-butoxycarbonyl)-4-(6-bromonaphthalene-2-sulfonyl)piperazine (2.80 g) were added methanol (10 ml) and 4 N hydrochloric acid in ethyl acetate solution (25 ml), and the solution was stirred at room temperature for 30 minutes. The reaction solution was concentrated and the residue was treated with acetone to give amorphous powders. The powders were dried under reduced pressure to give the title compound (2.358 g).

Workup

  1. concentrationThe reaction solution was concentrated
  2. additionthe residue was treated with acetone
  3. customto give amorphous powders
  4. customThe powders were dried under reduced pressure

Sources & evidence

ORD record
ord-f6570bd0ea31423cbc86ce14054fef79
Source dataset
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06359134B1

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes