Reference of 111-95-5,Some common heterocyclic compound, 111-95-5, name is Bis(2-methoxyethyl)amine, molecular formula is C6H15NO2, 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 Synthesis of DTPA bis(di(2-methoxyethyl-amide)(3) 12.4 ml of bis(2-methoxyethyl)amine (0.084 mol), dissolved in 40 ml of anhydrous DMF, are added dropwise to 5_grams of DTPA anhydride (0.014 mol), dissolved in 80_ml of anhydrous DMF, under argon at 80 C. The reaction medium is kept stirred for 24 hours.After concentrating and addition of diethyl ether, the oily precipitate is separated from the solvents by settling.This residue is dissolved in the minimum amount of CHCl3 and reprecipitated from Et2O. After drying under vacuum, a hygroscopic foam (3) is obtained (6.43 g, yield of 74%), used without additional purification. 1H NMR (D2O+NaOD): 2.50 (t, 4H), 2.52 (t, 4H), 2.98 (s, 2H), 3.11 (s, 4H), 3.31 (s, 6H), 3.32 (s, 6H), 3.51 (s, 4H), 3.53-3.56 (m, 16H).13C NMR (D2O): 45.94, 47.03, 47.81, 49.75, 53.69, 56.29, 57.78, 67.16, 69.56, 69.69 (CH2); 58.63, 59.07 (OCH3); 166.9, 170.5, 175.7 (CO2H and CO). ES-MS: ES-: 622.1 ([M-H]-), ES+: 624.3 ([M+H]+), 646.2 ([M+Na]+).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Bis(2-methoxyethyl)amine, its application will become more common.
Reference:
Patent; Lemaire, Marc; Foos, Jacques; Guy, Alain; Chitry, Frederic; Pellet-Rostaing, Stephane; Vigneau, Olivier; US2004/81604; (2004); A1;,
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