Application of 915095-86-2,Some common heterocyclic compound, 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, molecular formula is C13H7ClFIO, 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.
To a solution of the fluoride VIII.1 (208 kg), tetrahydrofuran (407 kg) and (S)-3-hydroxytetrahydrofuran (56 kg) is added potassium-tert-butanolate solution (20percent) in tetrahydrofuran (388 kg) within 3 hrs at 16 to 25¡ã C. temperature. After completion of the addition, the mixture is stirred for 60 min at 20¡ã C. temperature. Then the conversion is determined via HPLC analysis. Water (355 kg) is added within 20 min at a temperature of 21¡ã C. (aqueous quench). The reaction mixture is stirred for 30 min (temperature: 20¡ã C.). The stirrer is switched off and the mixture is left stand for 60 min (temperature: 20¡ã C.). The phases are separated and solvent is distilled off from the organic phase at 19 to 45¡ã C. temperature under reduced pressure. 2-Propanol (703 kg) is added to the residue at 40 to 46¡ã C. temperature and solvent is distilled off at 41 to 50¡ã C. temperature under reduced pressure. 2-Propanol (162 kg) is added to the residue at 47¡ã C. temperature and solvent is distilled off at 40 to 47¡ã C. temperature under reduced pressure. Then the mixture is cooled to 0¡ã C. within 1 hr 55 min. The product is collected on a centrifuge, washed with a mixture of 2-propanol (158 kg) and subsequently with tert.-butylmethylether (88 kg) and dried at 19 to 43¡ã C. under reduced pressure. 227 kg (91.8percent) of product are obtained as colourless solid. The identity of the product is determined via infrared spectrometry.
The synthetic route of 915095-86-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237789; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com