Hydrochloric Acid → HCID 21473495, compound

HRID 2294146Notes

Reaction equation

HRID 2294146 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]2[C:29]([CH3:30])=[CH:28][CH:27]=[CH:26][C:20]=2[C:21]([N:23]([CH3:25])[CH3:24])=[O:22])[CH2:11][CH2:10]1.[ClH:31].C(OCC)(=O)C>CO.C(Cl)Cl.CO>[ClH:31].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19]2[C:29]([CH3:30])=[CH:28][CH:27]=[CH:26][C:20]=2[C:21]([N:23]([CH3:24])[CH3:25])=[O:22])[CH2:11][CH2:10]1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 21473427HCID 21473427, compound

Product 1

HCID 21473495HCID 21473495, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 21226129Dichloromethane methanolSolvent

Procedure

A solution of 2-{3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamino}-N,N,3-trimethylbenzamide (70 mg, 0.17 mmol) in 0.5 mL of 5% methanol/methylene chloride was acidified with 0.6 mL of 1M hydrochloric acid in methanol and then ethyl acetate was added to give a precipitate. The supernatant was decanted and the precipitate was washed with ether, collected and dried to give 2-{3-[4-(2-methoxyphenyl)piperazin-1-yl]propylamino}-N,N,3-trimethylbenzamide hydrochloride (75 mg, 0.15 mmol). Anal.: Calcd. for C24H34 N4O2.(HCl)2.(H2O)0.5 : C, 58.53; H, 7.57; N, 11.38%; Found: C, 58.52; H, 7.68; N, 10.99%.

Workup

  1. customto give a precipitate
  2. customThe supernatant was decanted
  3. washthe precipitate was washed with ether
  4. customcollected
  5. customdried

Sources & evidence

ORD record
ord-5ca767b8846a40aba869234eafddb4ae
Source dataset
uspto-grants-1997_11
Patent number
US05688795

Reaction notes

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