Hydrochloric Acid → HCID 22676859, compound

HRID 1006238Notes

Reaction equation

HRID 1006238 reaction equation
[CH3:1][O:2][C:3]1[C:7]([CH3:8])=[C:6]([O:9][CH3:10])[S:5][C:4]=1[C:11]1[CH:51]=[CH:50][C:14]([C:15]([N:17]2[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][CH2:25][N:26]3[CH2:31][CH2:30][N:29]([C:32](=[O:49])[C:33]4[CH:38]=[CH:37][C:36]([C:39]5[S:40][C:41]([O:47][CH3:48])=[C:42]([CH3:46])[C:43]=5[O:44][CH3:45])=[CH:35][CH:34]=4)[CH2:28][CH2:27]3)[CH2:19][CH2:18]2)=[O:16])=[CH:13][CH:12]=1.C(OCC)(=O)C.[ClH:58]>C(Cl)(Cl)Cl>[ClH:58].[ClH:58].[CH3:45][O:44][C:43]1[C:42]([CH3:46])=[C:41]([O:47][CH3:48])[S:40][C:39]=1[C:36]1[CH:35]=[CH:34][C:33]([C:32]([N:29]2[CH2:30][CH2:31][N:26]([CH2:25][CH2:24][CH2:23][N:20]3[CH2:21][CH2:22][N:17]([C:15](=[O:16])[C:14]4[CH:50]=[CH:51][C:11]([C:4]5[S:5][C:6]([O:9][CH3:10])=[C:7]([CH3:8])[C:3]=5[O:2][CH3:1])=[CH:12][CH:13]=4)[CH2:18][CH2:19]3)[CH2:27][CH2:28]2)=[O:49])=[CH:38][CH:37]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 22676860HCID 22676860, compound

Product 1

HCID 22676859HCID 22676859, compoundYield 71%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

To a solution of 136 mg (0.173 mmol) of 1,3-bis[4-[4-(3,5-dimethoxy-4-methylthiophenyl)benzoyl]-1-piperazinyl]propane in chloroform (3 mL) stirred in an ice bath was added 0.11 mL (0.44 mmol) of a 4 mol/L ethyl acetate solution of hydrogen chloride, and the mixture was concentrated under reduced pressure. Methanol-diethyl ether was added and the precipitates were pulverized and collected by filtration to afford 105.0 mg of 1,3-bis[4-[4-(3,5-dimethoxy-4-methylthiophenyl)benzoyl]-1-piperazinyl]propane dihydrochloride as a colorless amorphous powder (yield 71%).

Workup

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionMethanol-diethyl ether was added
  3. filtrationcollected by filtration

Sources & evidence

ORD record
ord-e9ce331a982b4c579f5bb11919f6c558
Source dataset
uspto-grants-2004_09
Patent number
US06787653B2

Reaction notes

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