Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., Safety of 5-Fluoro-2-iodobenzoic acid
The 5-fluoro-2-iodo-benzoic acid by adding 13.87mol/L thionyl chloride in a solvent, heating to 60 C, stirring sleepovers Go fully clarified, TLC (PE/EA:10/1) monitoring after the reaction, to evaporate the solvent, adding toluene to dryness, ethyl acetate to dissolve the spare. 3658 g of diethyl malonate was added to 55 L of ethyl acetate, and 4762 g of magnesium chloride was added thereto at room temperature for 30 minutes. 4877 g of triethylamine was added dropwise, and the mixture was stirred for 30 minutes and cooled to 5 C. (5L X 2) was added under ice-cooling, and the organic phase was washed with saturated brine (10 L X), and the mixture was stirred at room temperature for 2 hours. TLC (PE / EA: 10/1) 2) Wash, separate and evaporate the organic layer to give a red oil. Add 12L of a mixture of acetic acid: water: concentrated sulfuric acid volume ratio of 6.6: 4.4: 1, heated to 100 C, stirred overnight (30LX 1), saturated brine (10 L X 2), dried and evaporated to dryness to give a red color. The organic phase was washed with 0.5N sodium hydroxide solution (30 LX 1) and saturated brine (10 L X 2) The product was obtained by passing the superfine silica gel column (PE / EA: 8/1)3.6Kg 1- (5-fluoro-2-iodophenyl)ethanone having the structural formula shown in Formula 3:
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; WuhanPharmaceutical Technology (Shanghai) Co., Ltd.; Guo, SongPo; Qiu, dongcheng; (9 pag.)CN105732355; (2016); A;,
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