Reaktion #1835507

Reaktionsgleichung

MeI

2-nitro-1H-imidazole

cesium carbonate

→

title compound

Ausbeute 86.7%

1-methyl-2-nitro-1H-imidazole

Ausbeute 86.7%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting suspension is cooled to room temperature
2. 2
   TemperaturThe reaction is heated to 50° C. for 2 hours
3. 3
   Temperaturis then cooled to room temperature
4. 4
   Filtrationfiltered through a bed of Celite
5. 5
   workup.ADDITIONThe filtrate is poured over ice water
6. 6
   Extraktionextracted ethyl acetate
7. 7
   WaschenThe organic layer is washed with water, brine
8. 8
   Trocknendried (Na2SO4)
9. 9
   Einengenconcentrated

Vorschrift

To a solution of 2-nitro-1H-imidazole (500 mg, 4.4 mmol) in DMF (50 mL) is added cesium carbonate (1.7 g, 5.3 mmol) and the mixture is heated to 50° C. for 30 minutes. The resulting suspension is cooled to room temperature and MeI (0.33 mL, 5.3 mmol) is added. The reaction is heated to 50° C. for 2 hours is then cooled to room temperature and filtered through a bed of Celite. The filtrate is poured over ice water and extracted ethyl acetate. The organic layer is washed with water, brine, dried (Na2SO4) and concentrated to afford the title compound (485 mg, 86%) as a yellow solid.

Quelle