A novel and one pot process for preparation of Nimorazole comprising the condensation of 4(5)-nitroimidazole (II) with 2-chloroethylmorpholine (III) in presence of potassium carbonate in toluene at reflux temp to yield N-2-morpholinoethyl-5-nitroimidazole (1) and N-2-morpholinoethyl-4-nitroimidazole (IV) and followed by in-situ salt preparation using maleic acid and further purification by crystallization of N-2-morpholinoethy]-5-nitroirnidazole (I) in methanol followed by treatment with ammonia in methanol to form Nimorazole having purity more than 99.0%