Réaction #9022
ord-f311fc80c113400083d5a3966db9b7c5
Équation de réaction
Réactifs
Aucun
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Températureto reflux for 3 hours
- 2Autreto precipitate a yellow solid
- 3Autrebottom of the flask (overnight)
- 4Autrethe supernatant solution was decanted
- 5AutreThe solid was dried under vacuum
Mode opératoire
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).