Ethyl Acetoacetate → HCID 178429174, compound

Participants

Reaction Steps

50 g of 4-nitro-2H-pyrazol-3-ylamine hydrochloride (prepared in accordance with H. Dorn and H. Dilcher, Liebigs Ann. Chem., 707, 141, 1967) and 60 g of ethyl acetoacetate in 160 cc of acetic acid were introduced into a 500 cc three-necked round-bottomed flask equipped with a magnetic stirrer, a thermometer and a condenser. The reaction medium was refluxed for 12 hours. The precipitate which formed was filtered off at about 90° C. It was washed with diisopropyl ether and dried under vacuum over phosphoric anhydride. This gave 50 g of 3-nitro-5-methylpyrazolo[1,5-a]pyrimidin-7-ol in the form of yellow crystals (yield=84.5%; melting point=290° C. with decomposition), whose elemental analysis, calculated for C7H6N4O3 (MW=194.15 g), was as follows:

Provenance & Evidence