Electric Literature of 150-78-7,Some common heterocyclic compound, 150-78-7, name is 1,4-Dimethoxybenzene, molecular formula is C8H10O2, 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.
Silfen was freshly prepared by thoroughly grindingFe(NO3)3(H2O)9 (2.0 g) and silica gel (4.0 g; 230-400 mesh) in a mortar [2]. A 25 mLround-bottomed flask was charged with 600 mg of silfen, iodine (142 mg; 1.1 mmol),1,4-dimethoxybenzene (138 mg; 1.0 mmol) and CH2Cl2 (2 mL), and the mixture wasstirred at 25 C overnight. The product was isolated by partitioning the reaction mixturebetween ethyl acetate and water, followed by washing the organic layer with 5% aqsodium thiosulfate and water, and drying (Na2SO4). Concentration by rotary evaporationgave an oil which was purified by CombiFlash chromatography (silica gel; 0-30%CH2Cl2 in hexane over 20 min) to afford a colourless oil (161 mg; 61%). 1H-NMR(CDCl3, 500 MHz): 3.74 (s, 3H, OCH3), 3.81 (s, 3H, OCH3), 6.74 (d, 1H, J = 8.8 Hz, H-6), 6.85 (dd, 1H , J = 8.8, 3.1 Hz, H-5), 7.30 (d, 1H, J = 3.1 Hz, H-3). 13C-NMR (CDCl3,125 MHz): 56.0, 57.1, 86.2, 111.7, 114.7, 125.0, 152.7, 154.3.
The synthetic route of 150-78-7 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Kempton, Robert J.; Kidd-Kautz, Taylor A.; Laurenceau, Soizic; Paula, Stefan; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 971 – 975;,
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