These common heterocyclic compound, 2752-17-2, name is 2,2′-Oxydiethanamine, 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: 2,2′-Oxydiethanamine
14.2) N,N’-(oxydiethane-2,1-diyl)bis(5-methoxy-4-nitro-1,3-benzothiazole-2-carboxamide) 3.03 g (6.5 mmol; 1.1 eq.) of bromo-tris-pyrrolidino-phosphonium hexafluorophosphate (PyBroP) is added to 1.5 g (5.9 mmol) of 5-methoxy-4-nitro-1,3-benzothiazole-2-carboxylic acid and 1.13 ml (6.5 mmol; 1.1 eq.) of diisopropylethylamine in solution in 100 ml of dichloromethane. The reaction mixture is maintained for 10 minutes under stirring at ambient temperature, then 0.31 g (2.9 mmol; 0.5 eq.) of 2.2′-oxybis(ethylamine) and a spatula tip’s worth of dimethylaminopyridine are added to the medium which is maintained under stirring for 18 hours at ambient temperature. The insoluble matter is filtered and the solvent is evaporated off under reduced pressure. The residue is then purified on a silica column (eluent:ethyl acetate/heptane: 4/1) and 250 mg of expected product (yield=8%) is obtained in the form of beige powder. MS-LC: MH+=577.11; r.t.=10.27 min.
The synthetic route of 2,2′-Oxydiethanamine has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Galcera-Contour, Marie-Odile; Prevost, Gregoire; Sidhu, Alban; US2007/244186; (2007); A1;,
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