66937-93-7Relevant articles and documents
Preparation method of argatroban intermediate esterified substance 4-methyl-2-ethyl piperidinecarboxylate
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Paragraph 0023; 0024; 0025; 0026; 0027; 0028; 0029-0040, (2017/10/07)
The invention relates to a preparation method of an argatroban intermediate esterified substance 4-methyl-2-ethyl piperidinecarboxylate. The preparation method comprises the following steps: adding a solvent, namely ethanol into a reaction kettle, putting a reactant, namely 4-methyl-2-piperidinecarboxylicacid hydrochloride into the reaction kettle, stirring to cool to (-5)-0 DEG C, maintaining the temperature, adding a catalyst, namely thionyl chloride, stirring to completely react until disappearance of raw material points is detected by virtue of a thin-layer chromatography, and carrying out vacuum reduced pressure concentration at 60 DEG C, so as to remove the solvent; and cooling the room temperature, adding dichloromethane, neutralizing reaction liquid by virtue of a 10% Na2CO3 solution, carrying out layered extraction, drying an organic solvent, and carrying out vacuum reduced pressure concentration at 50 DEG C on the organic solvent to remove the solvent, so as to obtain the esterified substance 4-methyl-2-ethyl piperidinecarboxylate. Mixed solvents including glacial acetic acid, ethanol and chloroform are replaced with single ethanol in a synthetic process, the reaction pressure is reduced, the catalyst thionyl chloride is low in cost, the operation is simple and convenient, the yield is substantially increased, and reaction solvents can be recycled, so that the preparation method is relatively beneficial to large-scale industrial production.
Direct diastereoselective synthesis of (±)-cis- and (±)-trans-4-methylpipecolic acid and derivatives
Cossy, Janine,Belotti, Damien
, p. 2119 - 2120 (2007/10/03)
(±)-cis- or (±)-trans-4-Methylpipecolic acid and ester derivatives can be obtained directly by addition of electrophiles to α-lithiated N-Boc 4-methylpiperidine.
HETEROCYCLIC THROMBIN INHIBITORS
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, (2008/06/13)
Heterocyclic thrombin inhibitors are provided which have the structure STR1 wherein n, R, R 1, R 2, R 3, G, G x, R. sup.6', Ra, Xa, R 6, Rb, R 3, p, Q, A and R 4 are as defined herein.