Sodium Hydroxide → HCID 178464037, Verbindung

HRID 1390022

Reaktionsgleichung

Reaktionsgleichung von HRID 1390022
[CH2:1]([N:3]([CH2:17][CH3:18])[CH2:4][CH2:5][N:6]1[C:10]2[N:11]=[C:12]([Cl:15])[CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[OH:16])[CH3:2].[Cl:19]([O-])(=O)=O.[K+].[OH-].[Na+]>Cl>[CH2:17]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]1[C:10]2[N:11]=[C:12]([Cl:15])[C:13]([Cl:19])=[CH:14][C:9]=2[N:8]=[C:7]1[OH:16])[CH3:18]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 6426889Potassium ChlorateHCID 178464036HCID 178464036, Verbindung

Produkt 1

HCID 178464037HCID 178464037, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
33 °C

Versuchsvorschrift

15 grams of 1-(2-diethylaminoethyl)-2-hydroxy-6-chloro-7-aza-benzimidazole were dissolved in 200 ml of concentrated hydrochloric acid and there were added in portions with stirring 24.5 grams of potassium chlorate at room temperature. The temperature increased temporarily to 33° C. The mixture was stirred for another hour, made alkaline with sodium hydroxide, the mixture extracted with shaking with n-butanol, the extract evaporated in a vacuum and the residue chromatographed over silica gel. The reaction product was recrystallized from ethyl acetate. M.P. 137°-139° C.; Yield: 3 grams.

Aufarbeitung

  1. additionthere were added in portions
  2. extractionthe mixture extracted
  3. stirringwith shaking with n-butanol
  4. customthe extract evaporated in a vacuum
  5. customthe residue chromatographed over silica gel
  6. customThe reaction product was recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b3af77507a9447b2b79d28e48f76a33f
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04247556

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