Potassium Carbonate → HCID 178490740, Verbindung

HRID 1902869Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1902869
[ClH:1].[OH:2][N:3]1[CH2:7][CH2:6][NH:5][CH2:4]1.[OH-:8].C([N+:13]([CH2:22][CH2:23]CC)([CH2:18][CH2:19][CH2:20][CH3:21])CCCC)CCC.[Cl:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][N+:29]=1[O-].[C:35](=[O:38])([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[Cl:26][C:27]1[C:28]([O:38][CH3:35])=[CH:33][CH:32]=[C:31]([Cl:1])[C:30]=1[N:29]=[C:4]1[NH:5][CH2:6][CH2:7][N:3]1[O:2][CH2:23][C:22]1[CH:21]=[CH:20][CH:19]=[CH:18][N+:13]=1[O-:8]

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 2655032-(Chloromethyl)pyridine 1-oxideHCID 2723671Tetrabutylammonium HydroxideHCID 86738714HCID 86738714, Verbindung

Produkt 1

HCID 178490740HCID 178490740, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

19.0 g of 2-[2,6-dichloro-3-methoxyphenyl)imino]-1-hydroxyimidazolidine hydrochloride are suspended in 160 ml of toluene. There are added thereto successively 40 ml of a 40 percent solution of tetra-n-butylammonium hydroxide, 12.2 g of 2-chloromethyl-pyridine N-oxide and 250 ml of a saturated potassium carbonate solution. After 4 hours, the precipitated material is removed by filtration, washed with water and subsequently with ether and recrystallized from chloroform and ethanol. There is obtained 2-([{2-[(2,6-dichloro-3-methoxyphenyl)-imino]-1-imidazolidinyl}oxy]methyl)-pyridine 1-oxide of melting point 199°-200° C. The corresponding dihydrobromide melts with decomposition at 192° (methanol/acetonitrile).

Aufarbeitung

  1. additionThere are added
  2. customthe precipitated material is removed by filtration
  3. washwashed with water and subsequently with ether
  4. customrecrystallized from chloroform and ethanol

Quellen und Nachweise

ORD-Eintrag
ord-6cf84a8730594767b03967a90b7f1801
Quelldatensatz
uspto-grants-1982_12
Patentnummer
US04366160

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