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Preparation method of tegafur gimeracil oteracil impurity BCB

A technology of impurity and tegafur, which is applied in the field of preparation of BCB impurity of Sigiol, and achieves the effect of mild reaction conditions and simple process

Inactive Publication Date: 2017-08-25
INST OF PHARMACY SHANDONG PROV ACAD OF MEDICAL SCI
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  • Claims
  • Application Information

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Problems solved by technology

In order to calibrate the impurity BCB in the S-1 preparation, it is necessary to obtain pure BCB as a reference substance first, but in the synthesis of each component in the S-1 capsule and the relevant pharmacology and toxicology literature, there are very few reports on BCB, and only a few words are provided. to BCB, and about the synthesis of BCB, there are no literature patent papers to report its synthesis

Method used

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  • Preparation method of tegafur gimeracil oteracil impurity BCB
  • Preparation method of tegafur gimeracil oteracil impurity BCB
  • Preparation method of tegafur gimeracil oteracil impurity BCB

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Embodiment Construction

[0029] Starting materials molecular weight Feeding amount (g) Tegafur 200.17 20 Gimeracil 145 29 sodium hydroxide 40 1 ethanol 46 180 water 18 120

[0030] Into a 500mL three-necked flask, add 20g of tegafur, 29g of gimeracil and 1g of sodium hydroxide in sequence, then add 180g of ethanol and 120g of water, start stirring, raise the temperature to 55°C, the solution is a clear and transparent system, and keep warm for 75h. After the reaction, concentrate under reduced pressure at 40°C, distill off ethanol, add 200g of water to the residue, and then raise the temperature to 60°C to continue the reaction for 4h. After the reaction, continue to cool down to room temperature, filter, and collect the filter cake. Dry in a forced air oven at 50°C for 8 hours to obtain 35 g of powdery solid. Add 35 g of the above solid into 300 mL of dichloromethane, heat to reflux for 2 h, and after cooling down to room temperature, filter, co...

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Abstract

The invention discloses a preparation method of a tegafur gimeracil oteracil impurity BCB. The preparation method comprises the following steps: (1) carrying out reaction on gimeracil and tegafur in presence of a catalyst to obtain a mixture containing BCB and gimeracil; and (2) carrying out chromatographic separation to obtain a BCB impurity. The preparation method disclosed by the invention has the advantages that technology is simple, reaction conditions are mild, and a high-purity BCB product can be obtained.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and specifically relates to a preparation method of S-1 impurity BCB, the chemical name of which is 3,3'-(4-hydroxybutanyl-1,1-diyl)bis (5-chloropyridine-2,4-diol). Background technique [0002] S-1 capsule is an oral anticancer agent of fluorouracil derivatives, which includes tegafur (FT) and the following two types of modulators: gimeracil (CDHP) and oteracil (OXO). S-1 often contains the impurity 3,3'-(4-hydroxybutanyl-1,1-diyl)bis(5-chloropyridine-2,4-diol) (BCB), which is S-1 Unavoidable impurities in preparations are also one of the impurity items that must be calibrated in S-1 preparations. [0003] In the import quality standard of S-1 capsule preparation, BCB is clearly mentioned as a specific impurity to be controlled. In order to calibrate the impurity BCB in the S-1 preparation, it is necessary to first obtain pure BCB as a reference substance. However, in the synthesis o...

Claims

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Application Information

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IPC IPC(8): C07D213/69G01N30/02
CPCC07D213/69G01N30/02
Inventor 薛玉涛刘腾赵普石秀娟窦春水
Owner INST OF PHARMACY SHANDONG PROV ACAD OF MEDICAL SCI
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