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4-Chlorobenzenesulfonyl chloride → (3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine

HRID 41302
Notes
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Reaction equation

HRID 41302 reaction equation
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][N:3]1C(OC(C)(C)C)=O.C(N(CC)CC)C.[Cl:22][C:23]1[CH:28]=[CH:27][C:26]([S:29](Cl)(=[O:31])=[O:30])=[CH:25][CH:24]=1>C(Cl)Cl>[Cl:22][C:23]1[CH:28]=[CH:27][C:26]([S:29]([N:6]2[CH2:5][CH2:4][NH:3][C@H:2]([CH3:1])[CH2:7]2)(=[O:31])=[O:30])=[CH:25][CH:24]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 10262201tert-Butyl (2R)-2-methylpiperazine-1-carboxylate

Product 1

HCID 11630465(3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazineYield 78.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 1,1-dimethylethyl (2R)-2-methyl-1-piperazinecarboxylate (1.5 g, 07.5 mmol) in dry DCM (40 mL) was added triethylamine (2.59 mL, 18.8 mmol) and 4-chlorobenzenesulfonyl chloride (3.15 g, 10.5 mmol) and the reaction stirred at room temperature for 48 h. To the reaction was added resin supported-triamine (5 g) and the mixture stirred for 4 h. The reaction mixture was filtered and the filtrate washed with 0.5 M HCl (aq., 100 mL) followed by water (100 mL) before it was dried (MgSO4), filtered and the solvent removed in vacuo. The crude product was dissolved in DCM (40 mL) and TFA (10 mL) was added. The solution was stirred for 20 min. The solvent was evaporated and the residue tajen up in DCM (40 mL) and washed with 50% aqueous sodium bicarbonate (100 mL) followed by water (100 mL). The organic phase was dried (MgSO4), filtered and the solvent removed in vacuo to give the title compound (1.62 g).

Workup

  1. additionTo the reaction was added resin
  2. stirringthe mixture stirred for 4 h
  3. filtrationThe reaction mixture was filtered
  4. washthe filtrate washed with 0.5 M HCl (aq., 100 mL)
  5. dry with materialwas dried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent removed in vacuo
  8. dissolutionThe crude product was dissolved in DCM (40 mL)
  9. additionTFA (10 mL) was added
  10. stirringThe solution was stirred for 20 min
  11. customThe solvent was evaporated
  12. washthe residue tajen up in DCM (40 mL) and washed with 50% aqueous sodium bicarbonate (100 mL)
  13. dry with materialThe organic phase was dried (MgSO4)
  14. filtrationfiltered
  15. customthe solvent removed in vacuo

Sources & evidence

ORD record
ord-d72421402bcd411a95caa05e81703400
Source dataset
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08530478B2

Reaction notes

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