反応 #9022

反応方程式

pyrazole

dimethylcyanamide

HCl

→

title compound

収率 78.0%

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

収率 78.0%

溶媒

1,4-dioxane

ether

反応条件

後処理

1. 1
   温度to reflux for 3 hours
2. 2
   その他to precipitate a yellow solid
3. 3
   その他bottom of the flask (overnight)
4. 4
   その他the supernatant solution was decanted
5. 5
   その他The solid was dried under vacuum

実験手順

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).

出典