Electric Literature of 13468-02-5,Some common heterocyclic compound, 13468-02-5, name is N,N-Dimethyl-2-phenoxyethanamine, molecular formula is C10H15NO, 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.
Example 5 – Sodium 4-(2-dimethylaminoethoxy)-benzenesulfonate 7.00 g (42.4 mmol) of dimethyl-(2-phenoxyethyl)-amine were dissolved in 35 mL of glacial acetic acid and cooled in an ice bath. 9.63 g (93.3 mmol) of 95% sulfuric acid were dropped in while maintaining an internal temperature of 10C or lower followed by stirring for 1 hour at room temperature. The solution was concentrated followed by the gradual addition of the concentrated residue to 1 mol/L sodium hydroxide to bring pH10, after which the solution was concentrated and dried. After extracting the residue with methanol, concentrating and drying, the residue was suspended in 100 mL of ethanol followed by cooling and filtration. The filtrate was concentrated and the precipitated crystals were filtered to obtain 8.36 g of the target substance (yield: 74%). 1H-NMR (400 MHz, D2O): delta = 7.68 (d,2H,J=8.8 Hz), 7.01 (d,2H,J=8.8 Hz), 4.33 (t,2H,J=5.0 Hz), 3.53 (t,2H,J=5.2 Hz) 13C-NMR (400 MHz, D2O): delta = 158.12, 133.61, 125.61, 112.90, 61.79, 59.66, 41.70 IR (KBr): nu = 3431, 3097, 2770, 1599, 1180, 1032, 844 cm-1
The synthetic route of 13468-02-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Dainippon Ink and Chemicals, Incorporated; EP1736464; (2006); A1;,
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