تفاعل #9022

معادلة التفاعل

pyrazole

dimethylcyanamide

HCl

→

title compound

المردود 78.0%

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

المردود 78.0%

المذيبات

1,4-dioxane

ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux for 3 hours
2. 2
   أخرىto precipitate a yellow solid
3. 3
   أخرىbottom of the flask (overnight)
4. 4
   أخرىthe supernatant solution was decanted
5. 5
   أخرىThe solid was dried under vacuum

الإجراء التجريبي

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).

المصدر