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

HRID 565756
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 565756
[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.[C:34]([OH:39])(=[O:38])[C:35]([OH:37])=[O:36]>CO>[C:34]([OH:39])(=[O:38])[C:35]([OH:37])=[O:36].[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 15895709N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide

Produkt 1

HCID 22111595N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide oxalateAusbeute 71,8 %

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 (50 ml). Oxalic acid dehydrate (0.32 g, 2.55 mmol) was added thereto. After dissolving the mixture with heating, the solvent was removed by evaporation in vacuo. Acetone was added to the residue, and the precipitated crystals were collected by filtration. The crystals were recrystallized from acetone, to give N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide oxalate (0.85 g) as colorless crystals (yield based on N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide: 71.8%).

Aufarbeitung

  1. dissolutionAfter dissolving the mixture
  2. temperaturewith heating
  3. customthe solvent was removed by evaporation in vacuo
  4. additionAcetone was added to the residue
  5. filtrationthe precipitated crystals were collected by filtration
  6. customThe crystals were recrystallized from acetone
  7. customto give

Quellen und Nachweise

ORD-Eintrag
ord-31250b2ecc12462fab57b5aea4c1ed62
Quelldatensatz
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06172228B2

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