In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 120800-05-7, name is 1-(5,6-Dichloropyridin-3-yl)ethanone, the common compound, a new synthetic route is introduced below. Safety of 1-(5,6-Dichloropyridin-3-yl)ethanone
To a 50-mL round-bottomed flask was added l-(5,6-dichloro-3- pyridinyl)ethanone (700 mg, 3.68 mmol), cesium fluoride (28 mg, 0.18 mmol, Sigma- Aldrich, St. Louis, MO), and DME (8 mL). The reaction mixture was cooled to 0 C and under a nitrogen atmosphere (trifluoromethyl)trimethylsilane (0.65 mL, 4.42 mmol, Sigma-Aldrich, St. Louis, MO) was added. The reaction mixture was stirred at 0 C for 1.5 h and then carefully quenched by adding aqueous 5N HC1 (5 mL). The reaction mixture was stirred at room temperature for 18h. The reaction mixture was carefully diluted with saturated aqueous sodium bicarbonate (about 10 mL) and extracted with EtOAc (2 x 30 mL). The organic extract was washed with brine, dried (Na2S04), filtered, and concentrated in vacuum. The crude material was absorbed onto a plug of silica gel and purified by chromatography through a silica gel column (40 g), eluting with a gradient of 0 % to 10% EtOAc in hexanes, to provide 2-(5,6-dichloro-3-pyridinyl)- 1,1,1 – trifluoro-2-propanol (812 mg) as a colorless oil. 1H NMR (400 MHz, DMSO-d6) delta ppm 8.60 (d, J= 2.15 Hz, 1H), 8.27 (d, J = 2.15 Hz, 1H), 7.12 (s, 1H), 1.75 (s, 3H). (m/z (ESI, +ve ion) 260.0 (M)+.
The synthetic route of 120800-05-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; AMGEN INC.; ASHTON, Kate; BOURBEAU, Matthew, Paul; HONG, Fang-Tsao; LIU, Longbin; NISHIMURA, Nobuko; NORMAN, Mark, H.; POON, Steve, F.; STEC, Markian, M.; ST. JEAN, David, J., JR; TAMAYO, Nuria, A.; YANG, Kevin, C.; WO2013/123444; (2013); A1;,
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