Reacción #48022

Ecuación de reacción

4-nitro-1,2-phenylenediamine

cyclopropanecarboxylic acid

→

brown oil

Rendimiento 98.0%

2-Cyclopropyl-5-nitro-1H-benzimidazole

Rendimiento 98.0%

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaat reflux for 14 hours
2. 2
   ConcentraciónThe reaction mixture is then concentrated under reduced pressure
3. 3
   LavadoThe organic phase is washed with 100 ml of water
4. 4
   Secadowith 50 ml of saturated sodium chloride solution, dried over magnesium sulfate
5. 5
   Concentraciónconcentrated under reduced pressure

Procedimiento

By analogy with a described method (WO 96/04270), a solution of 5 g (32.65 mmol) of 4-nitro-1,2-phenylenediamine in 77 ml (0.979 mol) of cyclopropanecarboxylic acid is stirred at reflux for 14 hours. The reaction mixture is then concentrated under reduced pressure and taken up in 150 ml of ethyl acetate and 100 ml of sodium hydrogen carbonate. The organic phase is washed with 100 ml of water and then with 50 ml of saturated sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure. 6.5 g of a brown oil are obtained, and are used without further purification in the following step.

Fuente