Reacción #9022

Ecuación de reacción

pyrazole

dimethylcyanamide

HCl

→

title compound

Rendimiento 78.0%

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

Rendimiento 78.0%

Disolventes

1,4-dioxane

ether

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato reflux for 3 hours
2. 2
   Otroto precipitate a yellow solid
3. 3
   Otrobottom of the flask (overnight)
4. 4
   Otrothe supernatant solution was decanted
5. 5
   OtroThe solid was dried under vacuum

Procedimiento

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).

Fuente