- STEREOSELECTIVE SYNTHESIS AND PROCESS FOR THE MANUFACTURING OF 2'-DEOXYNUCLEOSIDES
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Methods for stereoselective synthesis and manufacturing of 2'-deoxynucleosides, such as 2'-ribonucleosides, are disclosed. In some embodiments, the 2'-deoxynucleoside is a β-anomer of 2'-deoxynucleoside having a 3' a hydroxyl, 4' β hydroxymethyl configuration. Nonlimiting examples of compounds prepared by the disclosed methods include 4'-thio-2'-deoxycytidine (T-dCyd) and 5-aza-4'-thio-2'-deoxycytidine (5-aza-T-dCyd; aza-T-dCyd; aza-T-dC).
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Page/Page column 33
(2019/08/26)
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- A 5 - azacytosine new synthesis method
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The invention discloses a 5 - azacytosine synthetic method, comprises the following steps: (1) to a sealed in the reaction device of a double-melamine, a ester, heating the reaction, distilling off the unreacted formic ester and corresponding after mellow,, to obtain white solid; (2) hydrochloric acid and ammonia refining step (1) the obtained product can be obtained after 5 - aza cytosine. The present invention in order to utilize high-pressure reactor, a ester and dicyandiamide direct reaction to synthesize 5 - aza cytosine. Wherein the formic acid ester at the same time as the reactant, the reaction solvent in the reaction process loop and the reaction of the dehydrating agent, so that the formic ester hydrolysis, dicyandiamide of hydration reaction of formic acid with the guanyl urea salt of the dehydration reaction under hydrothermal conditions can be operatively associated. Simplifies the synthesis process, to avoid the occurrence of side reactions, improves the product purity, the overall reaction yield to double-cyanamide idea is higher than 70%, purity higher than 98%.
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Paragraph 0036; 0037; 0038
(2019/01/08)
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- 5-azacytosine synthesis method
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The invention discloses a 5-azacytosine synthesis method .The method comprises the following steps that 1, dicyandiamide, formic acid and a catalyst p-toluenesulfonic acid are added into an airtight reaction device and heated to react to obtain emulsion matter; 2, the product obtained in the step 1 is refined through hydrochloric acid to obtain the 5-azacytosine .A high-pressure reaction kettle is utilized, under the p-toluenesulfonic acid catalysis condition, the dehydration reaction temperature of guanylurea formate is effectively lowered, anhydrous formic acid in a system is directly utilized as a dehydrating agent, the steps of a synthesis process are simplified, side reactions are reduced, the product quality is ensured, the productivity is improved, and reaction yield is higher than 80% based on dicyandiamide .
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Paragraph 0042; 0043; 0044; 0045; 0046; 0047; 0048-0079
(2017/07/20)
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- 5-azacytosine preparation method
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The invention relates to a preparation method for 5-azacytosine. The preparation method comprises: firstly reacting formic acid with a part of dicyandiamide at 50-60 DEG C, adding the residual dicyandiamide in batches after the reaction is steady, reacting at a constant temperature of 50-60 DEG C for 4 h, then heating to 100-110 DEG C and reacting for 1 h, adding acetic anhydride by dividing into two times, raising the temperature and performing refluxing reaction for 2 h, cooling to 60-70 DEG C, adding ethanol, continuing to cool to room temperature, filtering to obtain a 5-azacytosine crude product, then adding a mixed solution of ethyl acetate and ethanol, filtering and baking to dry, so as to obtain the 5-azacytosine finished product. The beneficial effects comprise that the prepared 5-azacytosine has the HPLC purity of 98.5% or more, has the impurity 1 content less than 0.5% and the impurity 2 content less than 0.1%, and the preparation method is good in technological safety, free of technological wastewater and suitable for large-scale industrialized production.
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Paragraph 0025; 0026; 0027; 0028
(2016/11/21)
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- An improved and scalable process for the synthesis of 5-azacytidine: An antineoplastic drug
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An improved, practical, and scalable process for the manufacture of antineoplastic drug, 5-azacytidine (1), is described. A thorough understanding of the reaction parameters and stability of the reaction intermediates led us to the development of a robust process. The challenges in the isolation and systematic approach used to streamline the process into a very robust and practical manufacturing process are described.
- Vujjini, Satish Kumar,Varanasi, Ganesh,Arevelli, Srinivas,Kandala, Sreenatha Charyulu,Tirumalaraju, Satyanarayana Raju,Bandichhor, Rakeshwar,Kagga, Mukkanti,Cherukupally, Praveen
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p. 303 - 306
(2013/04/10)
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- PROCESS FOR PREPARING AZACYTIDINE INTERMEDIATE
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The present invention provides a processes for preparing 5-Azacytidine, and intermediates thereof. The present invention further provides an analytical method for determining the purity of 5-Azacytidine in a sample.
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- AZACITIDINE PROCESS AND POLYMORPHS
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Processes for preparing azacitidine. Further included are processes for the preparation of crystalline azacitidine crystalline Form (I) and mixtures of azacitidine crystalline Forms (I) and (II).
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Page/Page column 29
(2010/04/03)
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- PROCESS FOR PREPARING AZACYTIDINE INTERMEDIATE
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The present invention provides a processes for preparing 5 -Azacytidine, and intermediates thereof, said process Comprising reacting a silylated 5-azacytosine of the formula (II), a sugar moiety having of the formula (III): and a protic acid; wherein R is a substituted or non substituted C1-C20 acyl moiety, R1, R2 and R3 are each independently H or an alkyl group, and X is a halogen. The present invention further provides an analytical method for determining the purity of 5-Azacytidine in a sample.
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Page/Page column 18
(2010/04/03)
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- Azacytosine analogs and derivatives
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Compounds and compositions of azacytosine analogs and derivatives are provided. In one aspect of the invention, analogs or derivatives of decitabine and azacitidine are provided with modification at the 4- and 6-position of the triazine ring, at the 1′-6′position of the ribose ring, or combinations thereof. Methods of synthesizing and manufacturing these analogs and derivatives are also provided. These compounds can be formulated into pharmaceutical compositions that can be used for treating any disease that is sensitive to the treatment with decitabine or azacitidine, such as hematological disorders and cancer.
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Page/Page column 4; sheet 3
(2008/06/13)
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- Process for the preparation of aqueous nicotinaldehyde
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A process for the preparation of an aqueous medium of nicotinaldehyde by the catalytic reduction of 3-cyanopyridine under hydrogen in the presence of Raney-nickel.
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- Process for the preparation of aminotriazine derivatives
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The present invention relates to a process for the preparation of aminotriazine derivatives of the formula I STR1 by the solvolysis of compounds of the formula II STR2 in the presence of gaseous hydrogen chloride in an alcoholic medium. The compounds of formula I are useful as intermediates in the manufacture of insecticides.
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