These common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, its 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. Recommanded Product: 7252-83-7
(1) Synthesis of 1-(2,2-Dimethoxyethylsulfanyl)-4-fluorobenzene In a nitrogen stream, 4-fluorobenzenethiol (2.5 ml, 23.4 mmol) and 2-bromo-1,1-dimethoxyethane (3.0 ml, 25.7 mmol) were added to a sodium methoxide methanol solution (0.5 M, 74.9 ml, 37.4 mmol) under cooling with ice and the reaction mixture was stirred at the same temperature for 10 minutes, and then heated and refluxed for five hours. The reaction mixture was concentrated under reduced pressure, and added with cold water. The mixture was extracted with ether. The organic layer was washed with a saturated sodium chloride aqueous solution, and then dried with sodium sulfate. After filtration, the solvent was distilled under reduced pressure, and the obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate: n-hexane (1:20)] to obtain the title compound (4.52 g, 89%). 1H-NMR (CDCl3) delta: 3.05 (2H, d, J=5.4 Hz), 3.35 (6H, s), 4.49 (1H, t, J=5.4 Hz), 6.85 (2H, t, J=9.0 Hz), 7.31 (2H, dd, J=8.7, 5.1 Hz)
The synthetic route of 2-Bromo-1,1-dimethoxyethane has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CHUGAI SEIYAKU KABUSHIKI KAISHA; EP1803721; (2007); A1;,
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