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Method for separating and purifying intermediate product of Valienamine bromide in effective Valiolamine synchronizing process

A technique for memeneamine bromide and synthesis process, which is applied in the field of separation and purification of an intermediate product effective memeneamine bromide, can solve the problems of complex process, uncontrollable substances, and high difficulty in purifying effective mememamine, and achieves a reasonable process. , Simple operation, short process effect

Inactive Publication Date: 2010-09-15
ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Takeda Pharmaceutical’s patent on the preparation of effective mycoholamine believes that it is necessary to prepare purified effective mycomolamine, and effective mycomolamine is not prepared by purifying effective mycomolamine. After bromination, the process substances cannot be controlled, and effective mycomolamine cannot separate
However, the purification of effective mycylamine is difficult, and the process of purifying effective mycylamine and then synthesizing effective mycylamine is relatively complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Pack 70L of YPR macroporous resin, regenerate with a mass ratio of 2% sodium hydroxide and 80% acetone aqueous solution, the dosage is 210L, the flow rate is 2BV / h, and then wash with deionized water until neutral, the amount of deionized water is 2-3 times the resin volume. After the bromination reaction was completed, 6.8kg of product bromide obtained by evaporating methanol to dryness was dissolved into 150L with deionized water, and then adsorbed on a macroporous resin. Collect the leaked liquid, and then wash with deionized water twice the volume of the resin to obtain 140L of bromide remaining on the resin, combine the leaked liquid and the cleaning liquid to a total of 290L, evaporate and concentrate under reduced pressure, and obtain a total of 5.8kg of purified bromide . The purified bromide was subjected to hydrogenolysis and ring-opening to obtain 850 g of the ring-opened product, namely effective mycodolamine crude product, and the main peak area was 82% as...

Embodiment 2

[0016] Pack 70L of YPR macroporous resin, regenerate with a mass ratio of 2% sodium hydroxide and 80% acetone aqueous solution, the dosage is 210L, the flow rate is 2BV / h, and then wash with deionized water until neutral, the amount of deionized water is 2-3 times the resin volume. After the bromination reaction is completed, 6.5 kg of product bromide obtained by evaporating methanol to dryness is dissolved into 150 L with deionized water, and then adsorbed by a macroporous resin. Collect the leaked liquid, then wash with deionized water twice the volume of the resin to obtain 140L of bromide remaining on the resin, combine the leaked liquid and cleaning liquid to a total of 290L, and conduct vacuum evaporation to obtain a total of 5.5kg of purified bromide . The purified bromide was subjected to hydrogenolysis and ring-opening to obtain 858 g of the ring-opened product, namely effective mycodolamine crude product, and the main peak area was 82.7% as detected by liquid chroma...

Embodiment 3

[0018] Pack 70L of YPR macroporous resin, regenerate with a mass ratio of 2% sodium hydroxide and 80% acetone aqueous solution, the dosage is 210L, the flow rate is 2BV / h, and then wash with deionized water until neutral, the amount of deionized water is 2-3 times the resin volume. After the bromination reaction is finished, 6.3 kg of product bromide obtained by evaporating methanol to dryness is dissolved into 150 L with deionized water, and then adsorbed by a macroporous resin. Collect the leaked liquid, then wash with deionized water twice the volume of the resin to obtain 140L of bromide remaining on the resin, combine the leaked liquid and the cleaning liquid to a total of 290L, and conduct vacuum evaporation to obtain a total of 5.4kg of purified bromide . The purified bromide was subjected to hydrogenolysis and ring-opening to obtain 854 g of the ring-opened product, namely effective mycodolamine crude product, and the main peak area was 82.3% as detected by liquid chr...

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Abstract

The invention relates to a method for separating and purifying an intermediate product of Valienamine bromide in the Valiolamine synchronizing process. In the process of preparing the Valiolamine from validamycin by using biological pyrolysis and chemical synthesis, after Valienamine obtained by biological pyrolysis and the Valiolamine are subjected to amino-protection, a Valienamine bromide protective product can be brominated and a Validamine protective product cannot be brominated and a brominated product of the Valienamine and the Validamine amido protective product have polar difference; and an impurity of the Validamine amido protective product in the brominated product of the Valienamine can be removed by using a method for adsorbing and separating through YPR macroporous resin in water phase. The invention simplifies the process flow of synthesizing the Valiolamine by using an effective validamycin pyrolysis product of the Valienamine and is beneficial to controlling the process flow and improving the purity of a final product of the Valiolamine.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to a method for separating and purifying effective mycosylamine bromide, an intermediate product in the synthesis process of effective mycosylamine. Background technique [0002] Effective mycosanolamine is the core structure of pseudoaminosugar compound enzyme inhibitors. Many pseudoaminosidase inhibitor drugs, such as hypoglycemic drugs acarbose and voglibose, contain effective mycodolamine derivatives in their structures. At present, the production and application of effective mycosamine have attracted more and more attention. Effective mycylamine is also the composition structure of the biological pesticide effectivemycin. The C-N bond of effectivemycin is cracked by microbial enzymolysis to obtain effective mycylamine and effective mycamine, and effective mycylamine is obtained by chemical synthesis. Mycodolamine, effective mycodolamine can be used as...

Claims

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Application Information

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IPC IPC(8): C07C215/44C07C213/08C07C213/10
Inventor 裘国寅姚萍华常宏
Owner ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD