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Synthesis method of oteracil potassium

A synthesis method and technology of oteracil potassium are applied in the field of synthesis of oteracil potassium, can solve the problems of many impurities, low operation safety, low conversion rate, etc., and achieve simple reaction operation and simple and easy-to-obtain raw materials. , the effect of reducing production costs

Active Publication Date: 2020-01-07
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Aiming at the problems of low conversion rate, many impurities and low operation safety existing in the current preparation process, the present invention aims to provide a kind of product with simple operation, mild reaction conditions, high product yield, high purity and less pollution. Synthetic method suitable for industrialized production of oteracil potassium

Method used

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  • Synthesis method of oteracil potassium
  • Synthesis method of oteracil potassium
  • Synthesis method of oteracil potassium

Examples

Experimental program
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Effect test

Embodiment 1

[0040] At room temperature, add 2-aminocarboxamido-2-oxoacetic acid (13.20g, 0.10mol), urea (13.81g, 0.23mol), p-toluenesulfonic acid (0.086g, 0.50mmol), into ethanol (100mL) , heated to 50°C for 6 hours, cooled to 0°C, adjusted the pH to 5.5 with an aqueous solution of potassium hydroxide, stirred and grown the crystal for 2 hours, then suction filtered, and the filter cake was washed with cold purified water and cold absolute ethanol in turn to obtain oteracil Potassium, yield 94.64%, detected by HPLC, wherein t R =14.726min is oteracil potassium, with a purity of 99.965% and a maximum of 0.012% impurity.

Embodiment 2

[0042]At room temperature, add 2-aminocarboxamido-2-oxoacetic acid (13.20g, 0.10mol), urea (6.00g, 0.10mol), p-toluenesulfonic acid (0.086g, 0.50mmol), into ethanol (100mL) , heated up to 35°C for 4 hours, cooled to 0°C, adjusted the pH to 5.5 with an aqueous solution of potassium hydroxide, stirred and grown the crystal for 4 hours, then suction filtered, and the filter cake was washed with cold purified water and cold absolute ethanol in turn to obtain oteracil Potassium, yield 90.78%, detected by HPLC, wherein t R =14.735min is oteracil potassium, with a purity of 99.936% and a maximum of 0.014%.

Embodiment 3

[0044] At room temperature, add 2-aminocarboxamido-2-oxoacetic acid (13.20g, 0.10mol), urea (5.40g, 0.09mol), p-toluenesulfonic acid (0.086g, 0.50mmol), into ethanol (100mL) , heated up to 50°C for 4 hours, cooled to 0°C, adjusted the pH to 5.5 with an aqueous solution of potassium hydroxide, stirred and grown the crystal for 2 hours, then suction filtered, and the filter cake was washed with cold purified water and cold absolute ethanol in turn to obtain oteracil Potassium, yield 89.78%, detected by HPLC, wherein t R =14.723min is oteracil potassium, with a purity of 99.862% and a maximum of 0.014%.

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Abstract

The invention provides a synthetic method of oteracil potassium. The method comprises the following steps: adding 2-carbamoyl amino-2-oxyacetic acid, urea and a catalyst into a solvent at room temperature, carrying out heating cyclization reaction, detecting until the reaction is finished, cooling, adjusting the pH value of a reaction solution, forming a potassium salt, stirring, growing crystals,carrying out suction filtration, washing a filter cake with purified water and cold anhydrous alcohol in sequence, and carrying out vacuum drying to obtain oteracil potassium. Compared with the priorart, the method has the advantages of simple and easily available raw materials, simple operation, mild reaction conditions, stable quality, high yield, no pollution to the environment, and suitableness for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a synthetic method of oteracil potassium. Background technique [0002] The compound involved in the present invention is Potassium oxonate, also known as potassium oxonate, chemical name: 1,4,5,6-tetrahydro-4,6-dioxo-1,3,5- Potassium triazine-2-carboxylate, the chemical structural formula is as follows: [0003] [0004] Oteracil Potassium is one of the three active drugs in the oral anti-cancer compound drug T-Gio Capsules, which is an oral anti-cancer agent of fluorouracil derivatives, mainly composed of Tegafur and two biochemical regulators It is composed of gimeracil and oteracil potassium, of which tegafur has excellent oral bioavailability and can be converted into 5-fluorouracil in the body; gimeracil can inhibit the degradation of 5-fluorouracil, making 5-fluorouracil in plasma and tumor Maintain a stable blood concentration in the tissue fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/20
CPCC07D251/20
Inventor 张贵民朱安国刘东
Owner LUNAN PHARMA GROUP CORPORATION