According to the analysis of related databases, 17100-63-9, the application of this compound in the production field has become more and more popular.
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 17100-63-9 as follows. Safety of Methyl 4-bromo-3-methoxybenzoate
A suspension of methyl 4-bromo-3-methoxybenzoate (2.5 g; 10.2 mmol; 1.00 eq.), 4-methyl-3- thiopheneboronic acid (Aldrich 542393; 1.59 g; 11.2 mmol; 1.1 eq.), potassium carbonate (7.05 g; 51 mmol; 5 eq.) and Pd(PPh3)4 (1.18 g; 1 mmol; 0.1 eq.) in toluene (12.5 ml_) and water (12.5 ml.) was refluxed for 5 hours. The reaction mixture was cooled down to room temperature and filtered through a pad of celite which was further washed with touene (200 ml_). The filtrate was concentrated in vacuo and the residue taken up in Ethyl acetate (400 ml_). The organic layer was washed with sat. aq. NaHCC>3 (100 ml_), water (100 ml_) and brine (100 ml_) then dried over magnesium sulfate and concentrated in vacuo. The residue (2.3 g; 8.77 mmol; 1 eq.) was taken up in EtOH (69 ml_), sodium hydroxide (5M; 5.26 ml 26.3 mmol; 3 eq.) was added and the reaction mixture was stirred at 6O0C for one hour. After concentration in vacuo, the residue was taken up in water (200 ml_) and the aqueous phase was washed with Ethyl acetate then acidified to pH 2 with cone. HCI. The solution was concentrated to ca. 100 ml_ and the precipitate filtered off and dried to afford the title compound (1.81 g, 71 %) as a brown solid. HPLC (Method A) : Rt 3.99 min (purity 97.4%). LC/MS : 246.9 (M-H)”.
According to the analysis of related databases, 17100-63-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; MERCK SERONO S.A.; WO2009/43890; (2009); A1;,
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