161599-46-8Relevant articles and documents
Preparation method of capecitabine key intermediate
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Paragraph 0018; 0033; 0036-0037; 0038; 0041-0042, (2021/06/02)
The invention discloses a preparation method of a capecitabine key intermediate. According to the method, 2', 3', 5'-tri-0-acetyl-5-fluorocytidine servers as an initial raw material, selectively deacetylating through di-tert-butyl chlorotin hydroxide, and reducing through triethyl silane and trifluoroacetic acid to obtain a target product. The method has the advantages of cheap and easily available raw materials, short synthesis steps, simple operation, high product purity and high yield, and is especially suitable for industrial production.
Method for preparing capecitabine intermediate shown I
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Paragraph 0038-0049, (2019/08/21)
The invention discloses a method for preparing a Capecitabine intermediate represented by formula I. The method comprises the following reaction route shown in the description, wherein in the reaction a, 5-fluorocytosine reacts with hexamethyldisilazane to produce a compound represented by a formula III; in the reaction b, the compound represented by the formula III reacts with a compound represented by a formula II to produce the Capecitabine intermediate represented by the formula I; and in the general formula, R is H or a hydroxyl protecting group. According to the method, the high-yield preparation of the high-purity Capecitabine intermediate represented by the formula I is realized through strictly controlling the dropwise adding temperature and dropwise adding rate of Lewis acid, so that the subsequent preparation of high-purity Capecitabine is facilitated, and the requirements on industrialization of Capecitabine are met; and the method has a significant practical value.
Effective synthesis of nucleosides utilizing O-acetyl-glycosyl chlorides as glycosyl donors in the absence of catalyst: Mechanism revision and application to silyl-hilbert-johnson reaction
Liang, Chengyuan,Ju, Weihui,Ding, Shunjun,Sun, Han,Mao, Gennian
supporting information, (2017/01/24)
An effective synthesis of nucleosides using glycosyl chlorides as glycosyl donors in the absence of Lewis acid has been developed. Glycosyl chlorides have been shown to be pivotal intermediates in the classical silyl-Hilbert-Johnson reaction. A possible mechanism that differs from the currently accepted mechanism advanced by Vorbrueggen has been proposed and verified by experiments. In practice, this catalyst-free method provides easy access to Capecitabine in high yield.