Reaktion #671982

Reaktionsgleichung

5-bromo-2-methyl-4-nitroimidazole

mesitylboric acid

barium hydroxide octahydrate

→

title compound

Ausbeute 70.8%

Mesityl-2-methyl-4-nitro-1H-imidazole

Ausbeute 70.8%

Lösungsmittel

2,2-dimethoxyethane

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for four hours
2. 2
   FiltrationAfter filtered through Celite
3. 3
   workup.ADDITIONthe filtrate was diluted with ethyl acetate
4. 4
   Waschenwashed with brine
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   Sonstigeevaporated
7. 7
   WaschenThe resulting crystals were washed with ethyl acetate

Vorschrift

A solution of 5-bromo-2-methyl-4-nitroimidazole (5.0 g, 24 mmol), mesitylboric acid (3.96 g, 24 mmol), Pd(PPh3)4 (1.4 g, 1.2 mmol) and barium hydroxide octahydrate (19.1 g, 61 mmol) in 2,2-dimethoxyethane (150 mL) and water (25 mL) was heated at reflux for four hours. After filtered through Celite, the filtrate was diluted with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate and evaporated. The resulting crystals were washed with ethyl acetate, to give the title compound (4.17 g) as white crystals.

Quelle