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N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide → N-cyclopropyl-6-[-4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide dihydrochloride

HRID 565758
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 565758
[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1.[ClH:34].CO>CO>[ClH:33].[ClH:34].[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1
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Komponenten

4

Edukt 2

HCID 15895709N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamideHCID 21893726Hydrochloride methanol

Produkt 1

HCID 22111564N-cyclopropyl-6-[-4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

N-Cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide (1.00 g, 2.04 mmol) prepared in the same manner as in Example 1 was dissolved in methanol (10 ml). A 15% HCl-methanol solution was added thereto to make the solution acidic, and the solvent was then removed by evaporation in vacuo. Acetone was added to the residue, and the precipitated crystals were collected by filtration. The crystals were recrystallized from ethanol, to give N-cyclopropyl-6-[-4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide dihydrochloride (0.87 g) as colorless prisms (yield based on N-cyclopropyl-6-[-4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide: 75.7%).

Aufarbeitung

  1. customthe solvent was then removed by evaporation in vacuo
  2. additionAcetone was added to the residue
  3. filtrationthe precipitated crystals were collected by filtration
  4. customThe crystals were recrystallized from ethanol
  5. customto give

Quellen und Nachweise

ORD-Eintrag
ord-32ffb4f791364a31baeee8504def890d
Quelldatensatz
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06172228B2

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