Cycleanine production and purification method

A technology for the purification method of rennetin and its purification method, which is applied in the direction of organic chemistry, and can solve the problems that one-time crystallization cannot meet the product quality requirements of rennetin, many steps in the separation and purification process, and unfavorable industrialization, etc., so as to improve the safety of medication , reduce potential safety hazards, and mild process conditions

Active Publication Date: 2018-11-13
成都药云科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is that the separation and purification process operation steps of the existing phalloides product are many, loaded down with trivial details, and one-time crystallization can not reach the product quality requirements of the phalloides, and recrystallization is required. The purification yield is low, which is not conducive to industrialization

Method used

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  • Cycleanine production and purification method
  • Cycleanine production and purification method
  • Cycleanine production and purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1, the preparation of two imidazoline intermediate compounds

[0059] Add 200g of triethylenetetramine, 696g of toluene and 261g of DMF-DMA into the reaction vessel, heat to 85°C-105°C for reaction, separate methanol, continue to add to 120°C, separate 520g of toluene, and cool down to At room temperature, crystallize for 20 hours, filter, rinse the solid with toluene, and then dry it in vacuum at 30°C to obtain 128 g of a bis-imidazoline intermediate compound.

Embodiment 2

[0060] Embodiment 2, the preparation of bromide intermediate compound

[0061] Add 33.3g of potassium carbonate and 200mL of DMF into the reaction flask, stir and heat to 100°C, add 20g of bis-imidazoline intermediate compound, add 22.6g of dibromoethane and 600mL of DMF, and react the reaction solution at 100°C for 2 hours. After cooling down to 65°C, it was filtered, and the filtrate was concentrated under reduced pressure at 65-70°C and dried in vacuo to obtain a bromide salt intermediate compound (yellow semi-solid, 35.5 g).

Embodiment 3

[0062] Embodiment 3, the production and purification of the ring ring Teng Ning

[0063] Add 87g of potassium hydroxide and 100g of water to the reaction flask to obtain an aqueous potassium hydroxide solution, add 35.5g of the bromide salt intermediate compound to 140g of water to obtain an aqueous solution of the bromide salt intermediate compound, heat the potassium hydroxide aqueous solution to 105°C, and add bromine After the aqueous solution of the salt intermediate compound is kept warm for 1 to 2 hours, the reaction solution is cooled to 20°C for the first time, filtered, and the filtrate is cooled to 10°C for the second time to stand for crystallization for 24 hours, filtered and separated by filter cloth, and the solid is vacuum-dried at 30°C , to obtain Luhuan Tengning product (19.3g, yield 86.9%).

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Abstract

The invention discloses a cycleanine production and purification method which includes the steps: cooling cycleanine production reaction liquid for the first time; filtering the cycleanine productionreaction liquid; cooling filtrate for the second time and then performing standing, crystallization, filtering and drying to obtain a cycleanine product. According to the cycleanine production and purification method, cycleanine product post-treatment purification operation steps are simplified, hot filtration is omitted, the potential safety hazards of operators are reduced, production operationsafety level is reduced, and the method is green and environmentally friendly. The obtained cycleanine product is high in purity and good in quality, medication safety is improved, and industrialization is facilitated.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for the production and purification of trigonine. Background technique [0002] The compound rotenin, whose chemical name is 1,4,7,10-tetraazacyclododecane, is an organic synthesis intermediate, especially a precursor compound for the synthesis of metal ion macrocyclic chelating agents. For example, Rhizanthenin is used to synthesize gadobutrol as a contrast agent for MRI imaging of the brain and spinal cord, which can accurately determine the exact location of tumors and other lesions. There is great potential in the field of medical research. [0003] The existing published preparation methods of cyrthin include stetter method, Richman-Atkins method, Weisman method and oxalic acid condensation method. In the existing synthetic method, due to poor reaction selectivity, it is difficult to separate and purify tertenin. The quality and the yield of the overall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/02C07D487/22
CPCC07D257/02C07D487/22
Inventor 万家强
Owner 成都药云科技有限公司
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