Reference of 24878-25-9, These common heterocyclic compound, 24878-25-9, name is 2,2′-Oxydianiline, 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.
L. Nicotinic acid acyl azide and bis(2-aminophenyl) ether were synthesized according to previous literatures [24-26], respectively. A solution of nicotinic acid acyl azide (1.04?g, 7.0?mmol) in toluene (30?mL) was refluxed under nitrogen for 1.5?h, and bis(2-aminophenyl) ether (0.60?g, 3.0?mmol) in acetonitrile (30?mL) was added dropwise. The mixture was stirred for another 1.5?h and cooled to room temperature. The precipitate that formed was collected by filtration and purified by recrystallization from CH3OH/DMF(V: V?=?2:1) to give a white solid. Yield: 1.07?g, 81%; mp: 285???286?C. 1H NMR (DMSO-d6, 400?MHz): delta 6.84 (d, 2H, J?=?7.6?Hz, Ar-H), 7.02 (t, 2H, J?=?5.2?Hz, Ar-H), 7.18 (t, 2H, J?=?5.6?Hz, Ar-H), 7.36 (dd, 2H, J?=?2.8?Hz, Ar-H), 7.99 (m, 2H, Py-H), 8.23 (d, J?=?2.8?Hz, 2H, Py-H), 8.35 (d, J?=?6.8?Hz, 2H, Py-H), 8.61 (s, 2H, Py-H), 8.75 (s, 2H, CONH), 9.52 (s, 2H, CONH). 13C NMR (DMSO-d6, 400?MHz): delta 152.98, 145.76, 143.53, 140.33, 136.81, 131.60, 125.47, 124.64, 124.15, 123.20, 120.23, 118.38. Anal. Calcd(%) for C24H20N6O3: C 65.45, H 4.58, N 19.08; found(%): C 65.49, H 4.62, N 19.03. FT-IR (KBr pellet, nu/cm-1): 3344 (m, NH), 1715 (s, CO), 1599 (s, NH). ESI-MS: m/z?=?441 [M+H]+, 463 [M+Na]+.
The synthetic route of 24878-25-9 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Huang, Chao; Yi, Xian-Mei; Chen, Dong-Mei; Zhu, Bi-Xue; Inorganica Chimica Acta; vol. 476; (2018); p. 123 – 128;,
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