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Impurity in ubenimex bulk drug and preparation method of impurity

A technology of Ubenimex and raw material medicine, which is applied in the field of impurity and the preparation of the impurity, and can solve problems such as difficult quality control and difficult structure confirmation of Ubenimex raw material medicine

Inactive Publication Date: 2020-12-25
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the extremely small amount, it is difficult to collect and confirm the structure, which brings difficulties to the quality control of Ubenimex API

Method used

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  • Impurity in ubenimex bulk drug and preparation method of impurity
  • Impurity in ubenimex bulk drug and preparation method of impurity
  • Impurity in ubenimex bulk drug and preparation method of impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Synthesis of Example 1 Ubenimex bulk drug

[0047] Add 1000 mL of tetrahydrofuran into the three-necked flask, start stirring, add 100 g of Z-AHPA, 131.5 g of L-leucine benzyl ester p-toluenesulfonate and 48.5 g of 1-hydroxybenzotriazole (HOBt) in sequence, and then cool down to 0 ±2°C. Add 33.6g of triethylamine and 74.5g of dicyclohexylcarbodiimide (DCC), control the temperature at 12±2°C after the addition, stir and react for 20-24 hours, and filter the reaction solution after the reaction is complete. The filtrate was concentrated under reduced pressure until no distillate was evaporated to obtain an oily substance, and then ethyl acetate was added and stirred until the oily substance was completely dissolved. Wash the above ethyl acetate solution with 650 mL of 0.5 mol / L hydrochloric acid, 650 mL of purified water, 650 mL of saturated sodium bicarbonate solution, and 650 mL of saturated sodium chloride solution, respectively. The organic layer was dried by adding a...

Embodiment 2

[0052] The preparation of embodiment 2 formula I compound

[0053] i Weigh 20 g of Ubenimex and 11.0 g of sodium bicarbonate, add them to a glass reaction bottle, add 195 ml of water, 195 ml of tetrahydrofuran, stir, cool to 0, and add 11 g of benzyl chloroformate dropwise at 0 °C, the reaction temperature is 0- 4. ℃ after the dropwise addition was completed, the temperature was raised to room temperature and the reaction was continued overnight, 162 milliliters of water was added to the reaction solution, extracted twice with 162 milliliters of ethyl acetate, the two organic phases were combined, washed with 162 milliliters of saturated sodium chloride solution, and the organic phase was washed with 162 milliliters of saturated sodium chloride solution. Dry over anhydrous magnesium sulfate, filter, wash the filter cake with ethyl acetate, concentrate the filtrate to dryness under reduced pressure, add 100 ml of ethyl acetate, heat to dissolve, cool down to 0°C for crystalliza...

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Abstract

The invention provides an impurity generated in the preparation process of ubenimex bulk drug, and also provides a preparation method of the impurity. The purity of the impurity prepared by the methodreaches 99%, and the impurity can be used as a reference substance for the quality control process of the ubenimex bulk drug and preparation products of the ubenimex bulk drug.

Description

technical field [0001] The invention relates to the field of pharmaceutical synthesis methods, in particular to an impurity produced in the production process of ubenimex and a preparation method of the impurity. Background technique [0002] Ubenimex (Ubenimex; Bestatin) is a low-molecular-weight dipeptide compound isolated from the culture medium of Streptomyces olivine reticulum, which has the ability to inhibit tumor cell surface aminopeptidase B, N and leucine aminopeptide Enzyme action, inducing tumor cell apoptosis, promoting host cell immune function, and enhancing anti-cancer effect. It was launched in Japan in 1987. Ubenimex is often used in combination with other chemotherapy drugs in the treatment of acute myeloid leukemia, chronic myelogenous leukemia, lung squamous cell carcinoma, malignant melanoma, gastric tumor, etc.; combined with radiotherapy, it is used for nasopharyngeal carcinoma It is also used for the treatment of tumor diseases such as tumors, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/023C07K1/08
CPCC07K5/0202
Inventor 吴子强刘东华于玉根雷光华陈齐阳袁文
Owner 深圳万乐药业有限公司
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