Reference of 1187-42-4,Some common heterocyclic compound, 1187-42-4, name is Diaminomaleonitrile, molecular formula is C4H4N4, 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.
Under N2 atmosphere, bi-indole (420 mg, 1.4 mmol), diaminomaleonitrile (240 mg, 2.2 mmol) and sulfamic acid (1200 mg, 12.0 mmol) were refluxed in 30 mL of methanol for 3 h. The residual methanol was removed by vacuum distillation, then the resulting precipitate was washed by saturated aq. NaHCO3 and dried in vacuo to afford a yellow solid. The solid was subjected to chromatography over silica gel (ethyl acetate:petroleum ether, 1:1) to give 1 as yellow powder in about 80percent yield. 1H NMR (400 MHz, DMSO-d6, TMS): delta 7.10 (t, 2H, J = 7.3 Hz), 7.20 (t, 2H, J = 7.5 Hz), 7.48 (d, 2H, J = 8.0 Hz), 7.75 (d, 2H, J = 8.2 Hz), 7.81 (d, 2H, J = 2.4 Hz), 11.85 (s, 2H); ESI-MS (m/z): 359.2 [M?H]?, 394.6 [M+Cl]?, 754.5 [2M+Cl]?; HRMS (ESI) (m/z): 359.1047 [M?H]?, calcd. for C22H12N6 360.3709.
The synthetic route of 1187-42-4 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Liu, Xiu-Ming; Zhao, Qiang; Li, Yue; Song, Wei-Chao; Li, Ya-Ping; Chang, Ze; Bu, Xian-He; Chinese Chemical Letters; vol. 24; 11; (2013); p. 962 – 966;,
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