Reaktion #9022

Reaktionsgleichung

pyrazole

dimethylcyanamide

HCl

→

title compound

Ausbeute 78.0%

N,N-dimethyl-1H-pyrazole-1-carboxamidine hydrochloride

Ausbeute 78.0%

Lösungsmittel

1,4-dioxane

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 3 hours
2. 2
   Sonstigeto precipitate a yellow solid
3. 3
   Sonstigebottom of the flask (overnight)
4. 4
   Sonstigethe supernatant solution was decanted
5. 5
   SonstigeThe solid was dried under vacuum

Vorschrift

To a solution of pyrazole (1.01 g, 14.8 mmol) and dimethylcyanamide (1.20 mL, 14.8 mmol) in 1,4-dioxane (15 mL) was added HCl (4.0 N in 1,4-dioxane, 3.8 mL, 15.2 mmol) and the resultant mixture was heated to reflux for 3 hours. The reaction mixture was cooled to room temperature and diluted with dry ether (15 mL) to precipitate a yellow solid. The resultant precipitate was allowed to settle to the bottom of the flask (overnight) and the supernatant solution was decanted. The solid was dried under vacuum and provided the title compound (2.01 g, 78%). ES-MS m/z 139 (M+H).

Quelle