Related Products of 64115-88-4,Some common heterocyclic compound, 64115-88-4, name is 1-Bromo-2-(trifluoromethoxy)benzene, molecular formula is C7H4BrF3O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
5 rnL microwave vial was charged 4-ethynyl-7H-pyrrolo[2,3-d]pyrimidine (143 mg, 1.0 mmol), l-bromo-2-(trifluoromethoxy)benzene (241 mg, 1.0 mmol), PdCl2(PPhS)2 (35 mg, 0.05 mmol) and CuI (10 mg, 0.05 mmol). 3 mL of anhydrous CH3CN were added, after 10 min of stirring followed by 1.4 mL of Et3N. The reaction mixture was purged with argon for 5 min. Then the vial was capped and placed in a heating block at 60 0C for 18 h. Then it was cooled down to ambient temperature and concentrated in vacuo. The resulting black residue was re-dissolved in 3 mL of DMF and purified by reverse-phase preparative HPLC in CH3CN/H2O system containing 0.1% of TFA. Fractions, containing the product, were combined and partitioned between EtOAc (50 mL) and saturated aqueous NaHCO3 (50 mL). The organic layer was washed with brine (1 x 30 mL), dried over anhydrous Na2SO4 and filtered through a short silica gel plug. The filtrate was concentrated in vacuo to give the title product as a yellow solid (43 mg, 14% yield).[0334] 1H NMR (500 MHz, DMSO-J6): delta 6.63 (d, J = 3.5 Hz, IH), 7.55 (dt, J = 7.5, 1.0 Hz, IH), 7.59 (d, J = 8.4 Hz, IH), 7.67 (dt, J = 8.4, 1.7 Hz, IH), 7.75 (d, J = 3.5 Hz, IH), 7.92 (dd, J = 7.7, 1.6 Hz, IH), 8.79 (s, IH), 12.42 (s, IH)[0335] MS (ES+): m/z 304 (M+H)+
The synthetic route of 64115-88-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; TARGEGEN INC.; WO2009/55674; (2009); A1;,
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