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Hydrochloric Acid → HCID 178478870, Verbindung

HRID 1285335
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1285335
I.[CH2:2]([N:9]1[CH2:13][C:12](=[O:14])[N:11]=[C:10]1SC)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[N:17]1([CH2:23][C:24]2[CH:25]=[C:26]([CH:32]=[CH:33][CH:34]=2)[O:27][CH2:28][CH2:29][CH2:30][NH2:31])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.C(N(CC)CC)C.[ClH:42]>C(O)C>[ClH:42].[ClH:42].[N:17]1([CH2:23][C:24]2[CH:25]=[C:26]([CH:32]=[CH:33][CH:34]=2)[O:27][CH2:28][CH2:29][CH2:30][NH:31][C:10]2[N:9]([CH2:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[CH2:13][C:12](=[O:14])[N:11]=2)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 102205613-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amineHCID 20248961HCID 20248961, Verbindung

Produkt 1

HCID 178478870HCID 178478870, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

1-Benzyl-2-methylthio-2-imidazolin-4-one hydroiodide (2.09 g) from the previous stage, 3-(3-piperidinomethylphenoxy)propylamine (1.49 g) and triethylamine (1.27 g) were refluxed in ethanol (35 ml) for 7 hours with stirring. The solution was allowed to cool overnight and evaporated under reduced pressure to give a residue. This residue was dissolved in 2N hydrochloric acid (30 ml), and extracted with chloroform (3×20 ml). The aqueous layer was taken to pH 10 with 2N sodium hydroxide and extracted with chloroform (3×30 ml). The latter chloroform extracts were dried (MgSO4) and evaporated under reduced pressure. The residue was washed thoroughly with cold diethyl ether and treated with dilute ethanolic HCL. Excess solvent was evaporated and the residue recrystallised from isopropanolacetone to afford 2-[3-(3-piperidinomethylphenoxy)propylamino]-1-benzylimidazolin-4-one dihydrochloride, m.p. 95°-98° C.

Aufarbeitung

  1. temperatureto cool overnight
  2. customevaporated under reduced pressure
  3. customto give a residue
  4. extractionextracted with chloroform (3×20 ml)
  5. extractionextracted with chloroform (3×30 ml)
  6. dry with materialThe latter chloroform extracts were dried (MgSO4)
  7. customevaporated under reduced pressure
  8. washThe residue was washed thoroughly with cold diethyl ether
  9. additiontreated with dilute ethanolic HCL
  10. customExcess solvent was evaporated
  11. customthe residue recrystallised from isopropanolacetone

Quellen und Nachweise

ORD-Eintrag
ord-12fe3a3c0fc741e0a2435b6dacfae28f
Quelldatensatz
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04567176

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