Related Products of 347418-42-2, 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 347418-42-2 as follows.
Step 2 17.5 g Sodium hydride (60% dispersion in mineral oil) was suspended in300 ml N,N-dimethylformamide. The reaction mixture was cooled with an ice- water bath. 70.0 ml Diethyl malonate was added dropwise over 45 minutes. The resulting clear mixture was stirred at ambient temperature for 30 minutes. 36.2 g Crude product from the preceded step was added dropwise over 20 minutes at ambient temperature. The orange reaction mixture was stirred at ambient temperature. Reaction progress was monitored with HPLC. After 18 hours, the reaction mixture was concentrated in vacuo to remove most of the N,N- dimethylformamide.300 ml diethyl ether and100 ml water were added and the mixture was stirred vigorously for 5 minutes. The pH of the mixture was adjusted to ~7 with aqueous hydrochloric acid (1.5 M). The layers were separated and150 ml diethyl ether was added to the aqueous layer. The pH was again adjusted to ~7. The combined organic layers were washed with300 ml brine, dried (Na2S04) and concentrated in vacuo. The obtained yellow oily liquid contained still some mineral oil (floating on top). Most of the mineral oil was removed by using a separation funnel. The excess of diethyl malonate still present was removed by vacuum distillation (80C, 0.65 mbar). The product diethyl (5- fluoro-4-pyrimidinyl)malonate was isolated as a yellow oily liquid (89.6% purity acc. HPLC, NMR confirms expected structure) that was used directly in the next step.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,347418-42-2, its application will become more common.
Reference:
Patent; SYNTHRON B.V.; OVEREEM, Arjanne; ZHU, Jie; WO2011/110198; (2011); A1;,
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