Adding a certain compound to certain chemical reactions, such as: 213265-83-9, 4,6-Dichloro-5-fluoropyrimidine, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Quality Control of 4,6-Dichloro-5-fluoropyrimidine, blongs to pyrimidines compound. Quality Control of 4,6-Dichloro-5-fluoropyrimidine
Preparation 1 – 4-Chloro-5-fluoro-6-vinyl pyrimidine 5 A mixture of 4,6-dichloro-5-fluoropyrimidine (5.0 g, 30.0 mmol, 1.0 equiv) and tributyl(vinyl)tin (10.4 g, 33.0 mmol, 1.1 equiv) in dichloromethane(50 mL)was degassed with a stream of with nitrogen for 10 minutes. Bis(triphenylphosphine) palladium(ll) chloride (0.53 g, 0.75 mmol, 0.025 equiv) was added. The resulting mixture was degassed with a stream of nitrogen for an additional 15 minutes and heated at10 reflux for 72 hours. The reaction mixture was cooled to room temperature and quenched with an aqueous potassium fluoride solution (2 M, 75 mL, 5 equiv). The resulting mixture was allowed to stir for 2 hours and filtered through Celite. The filtrate was poured intoseparatory funnel and separated. The organic layer was washed with water (20 mL) and saturated brine (20 mL), dried over sodium sulfate, filtered and concentrated under15 reduced pressure at 20C. The resulting crude product was purified on an AnaLogix (SF40-i 1 5g) column. The gradient utilized for the purification was 10 minutes isocratic pentane, followed by a 20 minutes ramp to 5% diethyl ether in pentane. The pure fractions were combined and concentrated under reduced pressure at 20 C to give 4- chloro-5-fluoro-6-vinylpyrimidine (3.0 g, 63% yield).20+ 1Mass spectrum (positive mode): m/z 158.0 (M ). H NMR (300 MHz, CDCI3): oe (ppm)8.71 (s, 1H), 6.99 (m, 1H), 6.75 (dd, J=17.4 Hz, 1.8 Hz, 1H), 5.90 (dd, J=i0.5 Hz, 1.5 Hz, 1H). 19F NMR (282 MHz, CDCI3): oe 133.88 (s).
The synthetic route of 213265-83-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; PFIZER IRELAND PHARMACEUTICALS; BURRELL, Adam, James, Musgrave; O’NEILL, Padraig, Mary; PETTMAN, Alan, John; WO2014/60900; (2014); A1;,
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