Hydrochloric Acid → HCID 67117379, compound

HRID 1784676Notes

Reaction equation

HRID 1784676 reaction equation
[ClH:1].C(OCC)(=O)C.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]2[CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][C:17]([CH3:29])([CH3:28])[NH:16]2)=[CH:11][CH:10]=1>>[ClH:8].[ClH:1].[Cl:8][C:9]1[CH:10]=[CH:11][C:12]([CH:15]2[CH2:20][NH:19][CH2:18][C:17]([CH3:29])([CH3:28])[NH:16]2)=[CH:13][CH:14]=1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 67117378HCID 67117378, compound

Product 1

HCID 67117379HCID 67117379, compoundYield 95%

Procedure

4 M Hydrogen chloride in ethyl acetate (5.0 mL, 20.0 mmol) was added to a solution of 2-(4-chlorophenyl)-4-t-butoxycarbonyl-6,6-dimethyl-piperazine (1.69 g, 5.2 mmol). After 12 h, removing the solvent, filtrating and washing the precipitate with ethyl acetate gave 2-(4-chlorophenyl)-6,6-dimethyl-piperazine dihydrochloride (1.43 g, 95%). 1H NMR (300 MHz, DMSO-d6), δ 1.40 (3H, s), 1.58(3H, s), 3.24-3.99(4H, m), 4.73(1H, m), 7.69(2H, d, J=8.4 Hz), 7.79(2H, m), 9.99-10.12(2H, m).

Workup

  1. customremoving the solvent
  2. filtrationfiltrating
  3. washwashing the precipitate with ethyl acetate

Sources & evidence

ORD record
ord-9ad92844a8fe4dc194db8be14063770b
Source dataset
uspto-grants-2009_03
Patent number
US07504411B2

Reaction notes

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