Related Products of 499983-13-0, 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 499983-13-0 as follows.
Ethylene carbonate (370.2 g, 4.204 mol, 30.0 eq.) was loaded in a 500 ml reactor at room temperature and heated to an internal temperature of 40C till all the solid melted. Then 1.4 g of PEG-200 (0.007 mol, 0.05 eq.) and 30.0 g of 4-bromo-3-fluorophenylacetonitrile (0.140 mol, 1.0 eq.) were charged in the reactor. Potassium tert-butoxide (31.4 g, 0.280 mol, 2.0 eq.) was added portion-wise, under stirring, to the resulting clear colorless solution. The internal temperature rose up to 60C. Then, the mixture was heated to 130C and kept under stirring for 8 hours. The mixture was cooled to 40C and then 105 g of toluene and 240 g of deionised water were added. The mixture was kept under stirring for 15 minutes at 40C and then stirring was stopped. After 15 minutes two layers were separated: a lower organic clear red phase and an upper aqueous colorless phase. The organic solution was reloaded into the reactor and heated to an internal temperature of 40C. 240 g of deionised water were added. The mixture was kept under stirring for 15 minutes at 40C and then stirring was stopped. After 30 minutes the yellowish opalescent aqueous layer (lower) was discarded and the organic phase was washed again two times with 240 g of deionised water. After 30 minutes, the yellowish opalescent aqueous layer was discarded. The organic solution was warmed to 80C and the volatile solvents were removed under reduced pressure until 36 ml as the final volume. A solution 9.6 g of isopropyl alcohol was added. The solution was cooled from 80C to 50C in 30 minutes and a small amount of seed was added. The crystallization mixture was cooled from 50C to 0C in 60 minutes. The suspension was stirred for at least 60 minutes then filtered washing three times with 9.0 g of a toluene/isopropyl alcohol mixture (1/1.25 w/w). The wet product was dried under vacuum at 40C for 15-18 hours. 22.7 g of a pale yellow solid were obtained (purity = 99,94%; molar yield = 68%).
According to the analysis of related databases, 499983-13-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ZaCh System S.p.A.; Verzini, Massimo; Cotarca, Livius; Guidi, Alberto; Melloni, Alfonso; Maragni, Paolo; EP2818460; (2014); A1;,
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