Electric Literature of 1221171-96-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 1221171-96-5 as follows.
A 0.36 M solution of intermediate 6a in THF (42 mL, 15.12 mmol) was added to a stirred mixture of 4-bromo-2-methoxy-6-methylpyridine (CAS: 1083169-00-9; 2.98 g, 14.75 mmol) and Pd(/-Bu3P)2 (0.22 g, 0.31 mmol) at rt under N2. The mixture was stirred at reflux for 16 h. After cooling to rt a (1 : 1) mixture of a 32% solution of NFl·, (0369) (50 mL) and a saturated solution of NELCl (50 mL) was added. The mixture was extracted with EtOAc (200 mL). The organic layer was separated, dried (MgS04), filtered and the solvents were evaporated in vacuo. The crude product was purified by flash column chromatography (silica, EtOAc in heptane, gradient from 0/100 to 50/50). The desired fractions were collected and concentrated in vacuo to yield intermediate 7b as a colorless oil (4.34 g, 91%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1221171-96-5, its application will become more common.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose Manuel; TRABANCO-SUAREZ, Andres, Avelino; DE LUCAS OLIVARES, Ana Isabel; TRESADERN, Gary John; CONDE-CEIDE, Susana; (212 pag.)WO2019/243528; (2019); A1;,
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