914225-70-0, A common compound: 914225-70-0, name is 1-(5-Fluoro-2-iodophenyl)ethanone, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.
In a 500 mL reactor, 5-fluoro-2-iodoacetophenone (39.6 g, 150 mmol) was added.Glyoxylic acid monohydrate (13.9 g, 151 mmol), heating the reaction and distilling off water (95 , 0.1 Mpa) under reduced pressure for 3 hours.The reaction mixture was cooled to room temperature, 5% aqueous potassium carbonate solution (300 mL), and extracted twice with ethyl acetate,After 200 mL of water, the aqueous layer was acidified (10% hydrochloric acid, 300 mL), and then extracted twice with ethyl acetate.200 mL each time, the organic phase was combined, washed with brine and dried over anhydrous sodium sulfate.The solvent was removed under reduced pressure to give an orange solid.The solid was dissolved in glacial acetic acid (50 mL), concentrated hydrochloric acid (36%, 5mL).Acetic acid under reduced pressure, the residue was extracted (300 mL) with ethyl acetate, washed with brine three times,100 mL each time, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure.To give the desired product (26.89g, 56%) as a yellow solid, M.P.146 degrees.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-(5-Fluoro-2-iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Shanghai Health Medical School; Huang Gang; Li Bin; (101 pag.)CN109705124; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com