With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.2213-63-0,2,3-Dichloroquinoxaline,as a common compound, the synthetic route is as follows.
2-Amino-3-chloroquinoxaline (2a). The compound was synthesized by a slightly modified version of the procedure of Saikachi and Tagami [1] using a reaction temperature of only 80 C. Compound 1 (8.0 g, 40.2 mmol) was dissolved in N-methyl-2-pyrrolidinone (NMP) (60 mL) and heated to 80 ?C. Then, ammonia gas was bubbled through the hot solution for 3 h while the reaction was monitored by TLC. The crude product was poured into water (100 mL). The precipitate was collected by filtration, dried over CaCl2 and crystallized from chloroform to give 4.8 g (63%) pale yellow crystals, mp. 137-139 C. The NMR data are in accordance with a semihydrate. 1H-NMR (CDCl3): delta 1.85 (br, 1 H, 0.5 H2O), 5.53 (br s, 2 H, NH2), 7.47 (td, 3J = 8.3, 6.8, 4J = 1.7 Hz, 1 H, H-6), 7.63 (td, 3J = 8.3, 6.8, 4J = 1.4 Hz, 1 H, H-7), 7.69 (ddd, 3J = 8.3, 4J = 1.5, 5J = 0.5 Hz, 1 H, H-8), 7.86 ppm (ddd, 3J = 8.2, 4J = 1.3, 5J = 0.5 Hz, 1 H, H-5). 13C-NMR (CDCl3): delta 125.4 (CH-6), 126.1 (CH-8), 128.1 (CH-5), 130.6 (CH-7), 137.1, 137.3 (Cq-4a, Cq-3), 140.3 (Cq-8a), 148.7 ppm (Cq-2). MS (EI 70 eV, 165 ?C): m/z (%) = 181 (30) [M+(37Cl)], 179 (100) [M+(35Cl)], 144 (84), 117 (23), 102 (8), 90 (26), 44 (81). Water was separated by azeotropic distillation with toluene at normal pressure. Residual toluene was removed in vacuum. Anal. Calcd for C8H6ClN3 (179.61 gmol-1): C, 53.50; H, 3.37; N 23.40. Found: C, 53.59; H, 3.40; N 22.96.
2213-63-0, The synthetic route of 2213-63-0 has been constantly updated, and we look forward to future research findings.
Reference£º
Article; Adam, Mohamed Shaker S.; Mohamad, Ahmad Desoky; Jones, Peter G.; Kindermann, Markus K.; Heinicke, Joachim W.; Polyhedron; vol. 50; 1; (2013); p. 101 – 111;,
Quinoxaline – Wikipedia
Quinoxaline | C8H6N2 | ChemSpider