144301-85-9Relevant articles and documents
Iron-Catalyzed Radical Cleavage/C?C Bond Formation of Acetal-Derived Alkylsilyl Peroxides
Shiozaki, Yoko,Sakurai, Shunya,Sakamoto, Ryu,Matsumoto, Akira,Maruoka, Keiji
supporting information, p. 573 - 576 (2020/02/20)
A novel radical-based approach for the iron-catalyzed selective cleavage of acetal-derived alkylsilyl peroxides, followed by the formation of a carbon–carbon bond is reported. The reaction proceeds under mild reaction conditions and exhibits a broad substrate scope with respect to the acetal moiety and the carbon electrophile. Mechanistic studies suggest that the present reaction proceeds through a free-radical process involving carbon radicals generated by the homolytic cleavage of a carbon–carbon bond within the acetal moiety. A synthetic application of this method to sugar-derived alkylsilyl peroxides is also described.
Purification method of decitabine intermediate
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Paragraph 0038; 0039, (2020/07/24)
The invention belongs to the technical field of medicinal chemistry, and particularly relates to a purification method of a decitabine intermediate. The method comprises the following steps: dissolving a decitabine intermediate crude product in a first solvent such as trichloromethane, and adding a second solvent such as methyl tert-butyl ether, so that impurities generated in the synthesis process can be effectively removed, and the proportion of beta-configuration products can be increased when the refined intermediate is subjected to a glycosylation reaction.
Synthetic method of decitabine
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Paragraph 0044-0045, (2019/08/01)
The present invention relates to a synthetic method of decitabine, and discloses a method for synthesizing a compound as shown in a formula I, The method comprises the steps of: reacting a compound IIwith a compound III by a following reaction in a solvent under the action of TMSOTf to obtain a compound I. The synthetic method of the invention has the advantages that the raw materials are easy toobtain, the operation is safe, the conditions are mild and easy to control, and a solid product obtained by an acylation protection is easy to be crystallized and purified, which is favorable for thenext reaction and improves the selectivity of a final beta-isomer product, no further conversion to hydroxymethyl is required, the reaction step is simplified, the reaction yield of each step is good, the atomic economy is high, and the method is suitable for a large number of industrial production and the like.