Diethyl Ether → Pyridine-4-amidine hydrochloride

HRID 10237

Reaktionsgleichung

Reaktionsgleichung von HRID 10237
[Na].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)#[N:3].[Cl-:10].[NH4+:11].C(OCC)C>CO>[ClH:10].[C:2]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)(=[NH:11])[NH2:3]

Komponenten

6

Edukt 4

HCID 3283Diethyl EtherHCID 75064-CyanopyridineHCID 25517Ammonium ChlorideHCID 5360545Sodium

Produkt 1

HCID 2776844Pyridine-4-amidine hydrochlorideAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of sodium (0.23 g) in methanol (40 ml) was added 4-cyanopyridine (10.62 g) at r.t. Stirring was continued for 6 h followed by the addition of ammoniumchloride (5.9 g) and stirring was continued for another 10 h. Then, diethylether (120 ml) was added and the precipitate was filtered off after 30 min and washed with diethylether (20 ml). The product was dried under high vacuum. 4-Amidino-pyridine hydrochloride (14.95 g) was obtained as a white powder.

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for another 10 h
  3. filtrationthe precipitate was filtered off after 30 min
  4. washwashed with diethylether (20 ml)
  5. customThe product was dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-eabe532b36c040a6b450ec034d5b8835
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07094781B2

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