Synthetic Route of 1128-00-3, These common heterocyclic compound, 1128-00-3, name is Ethyl 2-aminocyclohex-1-enecarboxylate, 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.
In a 2000 ml flask were charged ethyl 2-aminocyclohexene-1-carboxylate (80.0 g, 472.8 mmol), pyridine (37.4 g, 472.8 mmol), and acetonitrile (190 ml), and the mixture was dissolved by heating to 40 C. While keeping the mixture at 40-50 C., a solution (126 ml) of benzyl chloride (63.14 g, 449.2 mmol) in acetonitrile was added dropwise. The mixture was stirred at 50-60 C. for 1.5 hr, cooled, and water (631 ml) was added dropwise at 20-30 C. over 30 min. After stirring at the same temperature for 30 min, the precipitate was collected by filtration and washed with water (631 ml). The obtained powder was dried under reduced pressure at 60 C. yield 119.62 g, 97%. [0533] Anal. calcd. for C16H19NO3, C, 70.31; H, 7.01; N, 5.12. found C, 70.29; H, 7.15; N, 5.08. HR-Ms calcd. for C16H19NO3, 274.1438 ([M+H]+). found, 274.1428 ([M+H]+).
The synthetic route of 1128-00-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Yamano, Mitsuhisa; Yamada, Masatoshi; Usutani, Hirotsugu; US2015/51416; (2015); A1;,
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