Hymexazol is an efficient and low-toxic soil fungicide.1 Hymexazol is commonly prepared by the condensation of hydroxylamine with ethyl acetoacetate using mineral acid derivatives under harsh reaction conditions.2 Recently, synthesis of hymexazol with commonly condensations has also been developed. Silica-supported boron trifluoride (BF3•SiO2) is the catalysts exhibit both Lewis and Brønsted acidity, Brønsted acidity in solid acid catalysts normally arises from polarised δ-O–Hδ+ sites and a Lewis acid center via an inductive effect of the electronegative F atoms on BF3. Many advantages such as inexpensiveness, uncomplicated handling, convenient work up, recyclability and insolubility in organic solvents, make BF3.SiO2 as an efficient catalyst in organic synthesis.3 In this paper, synthesis of hymexazol with combining of ethyl acetoacetate and hydroxylamine under new process with silica supported boron trifluoride catalyst (scheme. 1). Furthermore, the utilization of new process with silica supported boron trifluoride provides a good alternative for the synthesis of hymexazol and offers possibilities for industrial production.