1470-99-1Relevant articles and documents
Preparation method of Mitiglinide calcium intermediate
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Paragraph 0036-0044, (2018/11/22)
The invention relates to a preparation method of a Mitiglinide calcium intermediate. The method comprises the following steps: under nitrogen protection, adding tetrahydrofuran and zinc chloride intoa reactor in sequence for stirring, adding potassium borohydride one hour later, stirring for two hours, then adding cis-hexahydrophthalimide, carrying out a stirring reaction for two hours, adding asmall amount of concentrated sulfuric acid, slowly raising the temperature, heating to carry out a refluxing reaction for two hours, adding methylbenzene, slowly distilling until the internal temperature is about 94 DEG C, carrying out a refluxing reaction for three hours, continuously raising the temperature and distilling until the internal temperature is about 105 DEG C, stopping distillation,cooling below 30 DEG C, slowly dropwise adding 15% hydrochloric acid, after dropwise adding, raising the temperature and distilling until the internal temperature is about 107 DEG C, cooling below 30DEG C, dropwise adding 30% sodium hydroxide to adjust the pH value to be 13 to 14, and carrying out steam distillation and methylbenzene extraction drying to obtain cis-hexahydroisoindoline.
Enantioselective biocatalytic oxidative desymmetrization of substituted pyrrolidines
Koehler, Valentin,Bailey, Kevin R.,Znabet, Anass,Raftery, James,Helliwell, Madeleine,Turner, Nicholas J.
supporting information; body text, p. 2182 - 2184 (2010/06/18)
"Chemical Equation Presented" Center stage: Additions of nitrogen-centered radicals to cyanamide compounds provided the first radical synthesis of aromatic polycyclic guanidine derivatives (see scheme). Modular assembly of the substrates allows for a rapid increase of the molecular complexity of scaffolds, which have potential applications for medicinal chemistry.
Asymmetric desymmetrization of meso-pyrrolidine derivatives by enantiotopic selective C-H hydroxylation using (salen)manganese(III) complexes
Punniyamurthy,Katsuki, Tsutomu
, p. 9439 - 9454 (2007/10/03)
Chiral (salen)manganese(III) complexes 1 catalyzed the asymmetric desymmetrization of N-protected meso-pyrrolidine derivatives 3, 6-8, 15 and 18 by enantiotopic selective C-H oxidation in the presence of terminal oxidant iodosylbenzene. The oxidation occurred chemoselectively at the carbon α to the nitrogen atom to afford optically active hydroxypyrrolidine derivatives 9, 11, 13, 16, 19 and 21 that were further oxidized to chiral lactams with Jones reagent. The N-protecting groups of the meso-pyrrolidine derivatives have notable effect on the enantioselectivity.
