61367-07-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 61367-07-5 as follows.
(1) Methyl trans-4-aminocyclohexanecarboxylate hydrochloride (93.0 g) obtained in Reference Example 2(1) is dissolved in methanol (1000 ml), and thereto are added 35 % aqueous formaldehyde solution (95.4 ml), sodium acetate (39.4 g) and 10 % palladium/carbon (10 g). The mixture is then stirred at room temperature for 3.5 hours under atmospheric hydrogen pressure. The insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure. To the resulting residue is poured 20 % aqueous potassium carbonate solution (500 ml), and the mixture is extracted with chloroform. The organic layer is dried over sodium sulfate and potassium carbonate, and evaporated to remove the solvent under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: n-hexane/ethyl acetate = 2/1) to give methyl trans-4-dimethylaminocyclohexanecarboxylate (87.3 g). APCI-MS M/Z:186[M+H]+.;
According to the analysis of related databases, Methyl trans-4-aminocyclohexanecarboxylate hydrochloride, the application of this compound in the production field has become more and more popular.
Reference:
Patent; TANABE SEIYAKU CO., LTD.; EP1582521; (2005); A1;,
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