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. 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C15H14BrClO
Synthesis of compound 63C35H36F206/ C35H34F205I9F NMR (CDCU. 282.5MHz):Hydrate form: -1 17.3 (dd, Jl=257Hz, J2=30Hz, IF, CFF); -125.6 (d, Jl=258Hz, IF, CFF).Ketone form: -112.1 (ddd, Jl=260Hz, J2=32Hz, J3=6Hz, IF, CFF); -119.4 (dd, Jl=260Hz, J2=4Hz, IF, CFF).ass (ESf): 608.4 [M+H20]+; 613.5 [M+Na]+; 619.5 [M+K]+ To a solution of 62 (200mg; 0.35mmol; leq) in dry dichloromethane, under inert atmosphere, was added Dess-Martin periodinane (295mg; 0.70mmol; 2eq). The reaction medium was stirred for 3h at room temperature before a IN aqueous solution of sodium hydroxide (lOmL) was added. The aqueous layer was extracted with dichloromethane and dried over sodium sulphate, filtered and concentrated to afford ketone 63 (158mg, 77% yield) as a light orange solid which rapidly evolves toward the formation of the hydrate form until equilibrium is reached.Synthesis of compound 64C50H49CIF2O6 M=819.37g.mor1 19 F NMR fCDCk 282.5MHz): -1 12.3 (dd, Jl=266Hz, J2=27Hz, IF, CFF); -113.7 (dd, Jl=266Hz, J2=6Hz, IF, CFF).Mass (ESf): 836.7[M+H20]+; 841.8[M+Na]+; 857.7[M+K]+ In a Schlenk tube under inert atmosphere containing magnesium turnings (50mg, 2.04mmol, 1.2eq) was added 2inL (out of 5mL) of a solution of 10 (552mg, 1.70mmol, leq) and 1,2-dibromoethane (15mu, 0.17mmol, O. leq) in dry THF (5mL). The mixture was heated at 75C for 5 min to initiate the reaction and the last 3mL of the solution of 10 and 1,2-dibromoethane were then added dropwise at room temperature. This solution was then stirred at 75C for lh.2.4mL of this Grignard solution, previously cooled to room temperature, were then added to a solution of 63 (158mg, 0.27mmol) in dry THF (2mL). The reaction mixture was stirred at room temperature for 2h before a saturated aqueous solution of ammonium chloride was added. The aqueous layer was extracted with diethyl ether and the combined organic layers were washed with brine, dried over sodium sulphate, filtered and concentrated. The residue was purified on silica gel chromatography (cyclohexane/ethyl acetate 100:0 to 77:23) to afford compound 64 (152mg) as a mixture of two diastereomers with 69% yield. These diastereomers can be separated by semi- preparative HPLC.
The synthetic route of 461432-23-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; TFCHEM; DELIENCOURT-GODEFROY, Geraldine; LOPES, Lenaig; WO2012/160218; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics