As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 873107-98-3, name is 5-Iodo-2-(trifluoromethyl)pyridine, molecular formula is C6H3F3IN, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Application In Synthesis of 5-Iodo-2-(trifluoromethyl)pyridine
Step 2: ethyl 2,2-difluoro-2-(6-(trifluoromethyl)pyridin-3-yl)acetate [0252] To a solution of 5-iodo-2-(trifluoromethyl)pyridine (14.5 g, 53.2 mmol) and ethyl 2- bromo-2,2-difluoroacetate (10.8 g, 53.2 mmol) in DMF (250mL) was added Cu powder (6.76g, 106.4mmol). The mixture was heated to 80C for 20 hours. After 20 hours, the reaction mixture was poured into a solution of dibasic potassium hydrogen phosphate, trihydrate (121 g, 532 mmol) in water (1500 mL) with vigorous stirring. The suspension was filtered and the solid was rinsed with ether. The filtrate was added to brine and extracted with ether (2x). The combined organics were washed with brine, dried over sodium sulfate, filtered, and concentrated. The concentrate was purified by column chromatography over silica gel (hexane/EtOAc=50: l) to afford the title compound as a colorless liquid (8.96g, 63%). MS (ESI) calcd for CioH8F5N02: 269.2; found: 270.3 [M+H]. 1H NMR (400 MHz, CDCls) delta 8.98 (s, 1H), 8.14 (d, J= 8.2 Hz, 1H), 7.81 (d, J= 8.2 Hz, 1H), 4.35 (q, J = 7.1 Hz, 2H), 1.34 (t, J = 7.1 Hz, 3H).
With the rapid development of chemical substances, we look forward to future research findings about 873107-98-3.
Reference:
Patent; RUGEN HOLDINGS (CAYMAN) LIMITED; SHAPIRO, Gideon; (119 pag.)WO2015/187845; (2015); A1;,
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