Sodium Hydroxide → HCID 178478633, Verbindung

HRID 1581136Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1581136
[ClH:1].Cl.[CH3:3][NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1N.[C:12]([NH:14][C:15]([NH2:17])=[NH:16])#[N:13].[OH-].[Na+]>O>[ClH:1].[ClH:1].[NH:14]([C:12]1[N:4]([CH3:3])[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[N:13]=1)[C:15]([NH2:17])=[NH:16]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 178418324HCID 178418324, Verbindung

Produkt 1

HCID 178478633HCID 178478633, VerbindungAusbeute 42 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of N-methyl-o-phenylenediamine dihydrochloride (10.80g. 0.005 mol) and cyanoguanidine (9.30g, 0.11 mol) was heated under reflux in water (80 ml) for 21/2 hours. The reaction mixture was cooled, basified with excess 40% sodium hydroxide, and the resulting precipitate filtered, washed with water and dried in vacuo. (7.19g; m.p. 142°-146°C). This was dissolved in excess dilute hydrochloric acid and evaporated in vacuo. The crude hydrochloride was recrystallised from ethanol/ether to yield 2-guanidino-1-methylbenzimidazole dihydrochloride (600g; 42%) as off-white micro-crystals m.p. 228°-238°C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting precipitate filtered
  4. washwashed with water
  5. customdried in vacuo
  6. dissolutionThis was dissolved in excess dilute hydrochloric acid
  7. customevaporated in vacuo
  8. customThe crude hydrochloride was recrystallised from ethanol/ether

Quellen und Nachweise

ORD-Eintrag
ord-232650ec2c38446eacf20160de375e03
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03935314

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