Huang Ming-zhi
2006
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Journal
Fine Chemical Intermediates
Abstract
7-Fluoro-2H-1,4-benzoxazin-3(4H)-one(2) was prepared through the reaction of hydrogenization catalyzed by Rany Nickel from methyl 2-(5-fluoro-2-nitrophenoxy) acetate(1). The effect of temperature,catalyst,pressure of H2,reaction time,solvents and reclaim of all the solution and the catalyst were investigated. The optimum process conditions were determined as following:Reaction temperature was 70℃,time 4 h,the catalyst amount 5% comparing to 1 (w/w),the hydrogen pressure 5 MPa and methanol 1 000 mL/mol(1). The yield was 92.4% and the purity was 98%,all the solution and the catalyst could be reclaimed for four times and had no bad effect on the yield and purity. The structure of 2 was comformed by elementary analysis,IR,and 1H NMR.