Electric Literature 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.
EXAMPLE 2Cyclopropanation of 4-bromo-3-fluorophenylacetonitrile (II) with ethylene sulfate (III) to give 4-bromo-3-fluorophenyl-cyclopropanenitrile (IV)24 ml of lithium bis(trimethylsilyl)amide (1M in THF, 24 mmol, 2.2 eq.) were loaded at T=-20 C in a 50 ml dried reactor under nitrogen. 2.34 g of 4-bromo-3-fluorophenylacetonitrile (10.92 mmol, 1.0 eq.), dissolved in 5 ml of dry THF, and 1.49 g of ethylene sulfate (12.0 mmol, 1.1 eq.), dissolved in 5 ml of dry THF, were added in the reactor. The mixture was kept under stirring at T=-20 C. for 4 h and then heated to 20 C. The reaction was quenched by adding NH4Cl (saturated solution) and extracted with toluene. The organic layer was concentrated to dryness at reduced pressure to yield 3.01 g of crude product (assay=69.4%; molar yield=79.7%).
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; CHIESI FARMACEUTICI S.p.A; VERZINI, Massimo; Cotarca, Livius; Guidi, Alberto; Melloni, Alfonso; Maragni, Paolo; US2014/378696; (2014); A1;,
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