Oxalic Acid → HCID 178526031, Verbindung

HRID 486053

Reaktionsgleichung

Reaktionsgleichung von HRID 486053
[CH2:1]([N:9]=[C:10]=[S:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[NH:12]1[CH:16]=[C:15]([CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[N:14]=[CH:13]1.[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25]>C1(C)C=CC=CC=1.C(O)(C)C>[C:23]([OH:28])(=[O:27])[C:24]([OH:26])=[O:25].[CH2:1]([NH:9][C:10]([N:20]1[CH2:19][CH2:18][CH:17]([C:15]2[N:14]=[CH:13][NH:12][CH:16]=2)[CH2:22][CH2:21]1)=[S:11])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

Komponenten

6

Edukt 3

HCID 971Oxalic AcidHCID 16741Phenethyl IsothiocyanateHCID 1784208734-(1H-imidazol-4-yl)piperidine

Produkt 1

HCID 178526031HCID 178526031, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A solution of 1.63 g (0.01 mol) of phenethyl isothiocyanate in 60 ml of toluene and 1.51 g (0.01 mol) of 4-(4-imidazolyl)piperidine is heated to reflux for 1h 30 min. After cooling, the solution is evaporated under reduced pressure and the residual oil obtained is dissolved in 60 ml of isopropanol in the presence of 1.2 equivalents of oxalic acid. After 30 minutes of heating at 80° C., the white precipitate formed is drained, washed with ether and recrystallised in acetonitrile.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe solution is evaporated under reduced pressure
  3. customthe residual oil obtained
  4. customthe white precipitate formed
  5. washwashed with ether
  6. customrecrystallised in acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-474f4c34d56c412e9d2b44ede976dcb9
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05290790

Verknüpfte Notizen

Wird geladen…