In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2525-16-8, name is 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine
To a solution of ethyl N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-chloro-4-(piperidin-4-yloxy)phenyl]sulfamoylacetate dihydrochloride (0.75 g) obtained in example 47(a) in ethanol (25 ml) were added successively 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (0.39 g) and triethylamine (0.85 ml) at room temperature, and the resulting mixture was stirred at room temperature for 7 hours and then allowed to stand at room temperature for 15 hours.. Because of the slow progress of the reaction, 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (0.22 g) and triethylamine (0.51 ml) were furthermore added successively, and the resulting mixture was stirred at 45C for 12 hours, allowed to stand at room temperature for 11 hours and then furthermore stirred at 45C for 10 hours.. After stirring, to the reaction mixture was added a 4N solution of hydrogen chloride in dioxane (5 ml) and the resulting mixture was evaporated in vacuo.. The residue obtained was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 25 % acetonitrile/water).. Subsequently, to a solution of the amorphous solid obtained in ethanol (5 ml) was added a 4N solution of hydrogen chloride in dioxane (2 ml), and the resulting mixture was evaporated to dryness in vacuo.. The residue obtained was dissolved in water and then lyophilized to afford the title compound (0.30 g, yield: 35 %) as a colorless amorphous solid. 1H NMR (400MHz, DMSO-d6) delta ppm: 1.21 (3H, t, J=7.0), 1.52-1.63 (4H, m), 1.68-1.81 (4H, m), 2.04-2.10 (2H, m), 2.84-2.88 (2H, m), 3.36-3.42 (2H, m), 3.62-3.91 (4H, m), 4.18 (2H, q, J=7.0), 4.41 (2H, s), 4.46 (2H, d, J=6.0), 4.81-4.87 (1H, m), 6.44 (1H, dt, J=16.0, 6.0), 6.57 (1H, d, J=16.0), 7.32 (1H, d, J=9.0), 7.40 (1H, dd, J=9.0, 2.5), 7.52- 7.59 (2H, m), 7.66-7.74 (2H, m), 7.88 (1H, s); IR (KBr, cm-1): 1738, 1674, 1628, 1353, 1156.
The synthetic route of 2525-16-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Sankyo Company, Limited; EP1375482; (2004); A1;,
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