Réaction #9022

ord-f311fc80c113400083d5a3966db9b7c5

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températureto reflux for 3 hours
  2. 2
    Autreto precipitate a yellow solid
  3. 3
    Autrebottom of the flask (overnight)
  4. 4
    Autrethe supernatant solution was decanted
  5. 5
    AutreThe 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).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07091217B2uspto-grants-2006_08