论文部分内容阅读
以3-三氟甲基-4-腈基-苯胺和二硫化碳为原料制备异硫氰酸酯4-异硫氰基-2-三氟甲基苯腈(2),以2-氟-4-硝基甲苯为原料,经氧化、酰胺化、催化氢化制得N-甲基-2-氟-4-氨基苯甲酰胺(5),5与2-溴异丁酸乙酯反应得到2-(3-氟-4-甲胺甲酰苯基)胺基苯胺-2-甲基丙酸乙酯(6),2和6在无水N,N-二甲基甲酰胺溶液中缩合得到MDV3100(1),结构经MS和1H NMR确证,总收率18%(以2-氟-4-硝基苯甲酸计,n/n)。
Isothiocyanate 4-isothiocyanato-2-trifluoromethylbenzonitrile (2) was prepared starting from 3-trifluoromethyl-4-nitrile-aniline and carbon disulfide starting from 2- Nitrotoluene as raw material, after oxidation, amidation, catalytic hydrogenation N-methyl-2-fluoro-4-aminobenzamide (5), 5 and 2-bromoisobutyrate ethyl reaction 2- ( 4-Carbamoylphenyl) aminoaniline-2-methylpropanoate (6), 2 and 6 in anhydrous N, N-dimethylformamide to give MDV3100 1). The structure was confirmed by MS and 1H NMR with a total yield of 18% (n / n as 2-fluoro-4-nitrobenzoic acid).