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.
Preparation method of 2'-3'-bis-O-acetyl-5'-deoxy-5-fluoro-N4-[(pentyloxy)carbonyl]cytidine
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Paragraph 0020; 0061; 0062, (2017/08/28)
The invention relates to the field of pharmaceutical chemistry, in particular to a preparation method of 2'-3'-bis-O-acetyl-5'-deoxy-5-fluoro-N4-[(pentyloxy)carbonyl]cytidine; the method comprises: reacting a compound of formula IV as a raw material with n-amyl chloroformate under the action of K3PO4 to obtain the compound of formula V, 2',3'-bis-O-acetyl-5'-deoxy-5-fluorine-N4-[(pentyloxy)carbonyl]cytidine. The invention also provides application of the method in the preparation of capecitabine. The preparation method has the advantages that reaction yield can be significantly increased, product purity is high, reaction conditions are mild, the use of pyridine is avoided, pyridine residue in the product is avoided, and the method is suitable for industrial production of medicine.