Application of 52570-33-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 52570-33-9 name is Methyl 3-iodo-2-methylbenzoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Process using Pd Catalyst Under a nitrogen atmosphere, palladium acetate (223 mg, 0.99 mmol) , 4, 5-bis (diphenylphosphino) -9, 9-dimethylxanthene (Xantphos) (575 mg, 0.99 mmol) and toluene (62 ml) were mixed, and the mixture was stirred at room temperature for 15 minutes. To this solution, 2-amino-3-bromo-5-methylpyridine (6.20 g, 33.15 mmol), methyl 3-iodo-2-methylbenzoate (9.15 g, 33.15 mmol) and cesium carbonate (15.12 g, 46.41 mmol) were added. The mixture was stirred at an internal temperature of 100 to 105C for 7 hours. The reaction solution was cooled to room temperature, and water (50 ml) and toluene (50 ml) were added thereto. The organic layer was separated and washed sequentially with water (40 ml) and 10% brine (40 ml) . Silica gel (6 g) was added to the organic layer, the mixture was filtered, and the filtrate was concentrated under reduced pressure. Ethyl acetate (0.5 ml) and n-hexane (6 ml) were added to the concentrate, and the mixture was stirred at room temperature for 30 minutes. The crystals were collected by filtration, washed with ethyl acetate/n-hexane (1/12, 5 ml), and dried under reduced pressure at 40C, to yield the title compound (4.81 g) (yield 43.3%). 1H-NMR (CDCl3, TMS, 300 MHz) delta (ppm) : 2.23 (3H, s) , 2.52 (3H, s), 3.91 (3H, s), 6.78 (IH, brs) , 7.27 (IH, t, J = 8.0 Hz), 7.57-7.62 (2H, m) , 7.95 (IH, d, J = 1.1 Hz), 8.10 (IH, dd, J = 1.0 Hz, 8.1 Hz) .High resolution mass spectrometry Theoretical value: 334.0317 [M+] Measured value: 334.0313 [M+]Melting point: 63.9 to 64.7C
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-iodo-2-methylbenzoate, and friends who are interested can also refer to it.