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Preparation method of 5'-deoxidization-2',3'-diacetyl-5-fluoro-cytidine

A technology of flucytidine and diacetyl, applied in the field of 5'-deoxy-2', can solve the problem of high cost of anti-tumor drugs, achieve the effects of increased synthesis yield, accelerated reaction speed, and reduced manufacturing cost and price

Active Publication Date: 2011-05-11
ZHEJIANG CHENGYI PAHRMACEUTICAL
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  • Description
  • Claims
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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of high cost of existing antineoplastic drugs, to provide a more optimized 5'-deoxy-2', 3'-diacetyl-5-fluorocytidine preparation method, so that the yield is greatly improved Improve and save the synthesis cost of the final drug

Method used

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Embodiment 1

[0020] The three-necked flask equipped with a stepless speed-regulating stirrer, a thermometer of 0°C-150°C, and a reflux and can be turned into a distillation condenser is installed in an automatic constant temperature electric heating oil bath. Weigh 12.9g (0.10mol) of 5-fluorocytosine, put it into a three-neck flask, then put in 100ml of toluene, 22ml of hexamethyldisilazane, and 0.25g of ammonium sulfate, stir at high speed, raise the temperature above 100°C, and reflux for 3.5 After 1 hour, the toluene was distilled off under reduced pressure until the feed liquid was viscous, and a mixture of 24.5 g (0.094 mol) of 5-deoxy-1,2,3-triacetyl ribose and 120 ml of dichloromethane was added. Replace the oil bath with the low-temperature bath liquid of the low-temperature cooling circulation pump, cool the feed liquid to 0°C, add a mixed solution of 13ml of anhydrous tin tetrachloride and 30ml of dichloromethane, keep warm and stir at a slow speed for 3 hours. The reaction solut...

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Abstract

The invention belongs to the technical field of preparation methods of 5'-deoxidization-2',3'-diacetyl-5-fluoro-cytidine. The preparation method of the 5'-deoxidization-2',3'-diacetyl-5-fluoro-cytidine comprises the following steps: adding a silylating reagent and an additive of ammonia sulfate to 5-fluctyosine and reacting for 3 hours to 5 hours at 80 DEG C to 120 DEG C to distill part of reagent; then, adding 5'-deoxidization-1',2',3'-triacetyl ribose; and finally, cooling feed liquid to a temperature range from 0 DEG C-5 DEG C to 0 DEG C+ / -5 DEG C and adding anhydrous stannic chloride to continue a complete reaction. The ammonia sulfate is added when the reaction starts, takes obvious promotion effect on a reaction speed and carries out antidecomposition protection for sensitive components in the reaction so as to shorten the whole reaction time by 60 percent to 70 percent, improve the weight yield of a product by over 20 percent, enable the content to be larger than or equal to 98percent and directly greatly decrease the manufacture cost of the medicine.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of 5'-deoxy-2',3'-diacetyl-5-fluorocytidine. Background technique [0002] 5'-deoxy-2',3'-diacetyl-5-fluorocytidine is the basic raw material for the synthesis of anti-tumor drug "capecitabine" and so on. The chemical synthesis of nucleosides has been considered to be a relatively complex and difficult synthesis technology, and its synthesis process is still being explored and perfected by countless researchers. [0003] Invention patent representing the frontier technology of nucleoside drug synthesis: "N-oxocarboxyl substituted 5'-deoxy-5-fluorocytidine derivatives" (Chinese Patent Publication No. Regulations: Preparation of starting material, preparation of 2'-3'-diacetyl-5'-deoxy-5-fluorocytidine" column: "(b) with 5-fluorocytosine and 1,2,3-tris Acetyl-5-deoxy-β-D-ribofuranose as raw material" lists the preparation case: Add sodium iodide and molecular sieve 4A as additives in t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/06C07H1/00
Inventor 颜怡恰颜贻意岑均达
Owner ZHEJIANG CHENGYI PAHRMACEUTICAL
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