Synthetic Route of 641571-13-3,Some common heterocyclic compound, 641571-13-3, name is 3-(4-Methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)benzoic acid, molecular formula is C12H9F3N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
(VII) (10 g), t-butanol (300 mL), triethylamine (7.9 g) and diphenylphosphoryl azide (11.2 g) were added to a 500 mL reaction flask. The mixture was heated to reflux and refluxed for 16 hours then cooled to room temperature. The solvent was removed by evaporation under reduced pressure. The residue was treated with water (150 mL) and extracted with ethyl acetate (2 x 150 mL). The extracts were combined, washed with brine (150 mL), dried over sodium sulfate and evaporated to remove the solvent under reduced pressure to give the crude product (12.5 g).The above crude product (12.5 g), n-propanol (125 mL), p-xylene (125 mL) and solid sodium hydroxide (7.3 g) were added to a 500 mL reaction flask. The mixture was stirred and the mixture was heated to reflux and refluxed for 30 hours. Stirring was stopped, water (162 mL) was added and the azeotrope was distilled off under reduced pressure. The residue was diluted with water (20 mL), cooled to 0 & lt; 0 & gt; C, stirred slowly for 1 h and filtered. The filter cake was washed with water (2 x 30 mL) and dried in vacuo at 55 C to give 7.1 g of the solid compound (I). The HPLC purity was 98.7% and the overall yield of the two-step reaction was 79.5%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(4-Methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)benzoic acid, its application will become more common.
Reference:
Patent; Esteve Huayi Pharmaceutical Co., Ltd; Zhao, Liqiang; Wang, Zhao; Jiang, Hong; Dong, Jin; Xu, Xiaofei; Zheng, Guorong; (9 pag.)CN105985293; (2016); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem