The synthetic route of 2-Methoxy-N-methylaniline has been constantly updated, and we look forward to future research findings.
These common heterocyclic compound, 10541-78-3, name is 2-Methoxy-N-methylaniline, 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. HPLC of Formula: C8H11NO
To a stirring dichloromethane (40 mL) solution containing 5-bromo-4- chloro-2-hydroxybenzoic acid (2.0 g, 8.0 mmol), were added triethylamine (2.2 mL, 16.0 mmol), HATU (4.5 g, 12 mmol) and 2-methoxyl-N-methylaniline (1.19 g, 8.7 mmol). The mixture was stirred at rt for 16 hrs and water was added. The organic layer was separated, washed with NaHCO3, dried over Na2SO4, filtered and concentrated. The residue was purified via silica gel flash column chromatography eluting with 20% ethyl acetate in hexane to afford 5-bromo-4-chloro-2-hydroxy-N-(2- methoxy-phenyl)-N-methyl-benzamide (300 mg). MS [M+H]+: 371.9; tR = 2.60 min (method 1)Alternatively, a mixture of 5-bromo-4-chloro-2-hydroxybenzoic acid (5 g, 19.9 mmol), 2-methoxy-N-methyaniline (3.13g, 22.9 mmol) and P2O5 (5.36g, 37. 8 mmol) in anhydrous xylene was heated at 60 0C for 2 hrs and then refluxed for 17 hrs. The mixture was concentrated and purified via silica gel flash column chromatography eluted with ethyl acetate in hexane (20%) to give 5-bromo-4-chloro-2-hydroxy-N-(2- methoxy-phenyl)-N-methyl-benzamide (3.3 g).
The synthetic route of 2-Methoxy-N-methylaniline has been constantly updated, and we look forward to future research findings.
Reference:
Patent; NEUROCRINE BIOSCIENCES, INC.; WO2008/124610; (2008); A1;,
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