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Preparation method for 9-fluorenylmethoxycarbonyl succinimide

A technology of fluorenyl moxycarbonyl succinimide and fluorenyl moxycarbonyl chloride formate, applied in the field of preparation of 9-fluorenyl moxycarbonyl succinimide, can solve the problem of difficult separation, high production cost input, processing Low synthesis efficiency and other problems, to achieve the effect of meeting the needs of processing and synthesis, reducing production cost input, and simple equipment prices

Inactive Publication Date: 2013-10-16
TAICANG HENGYI MEDICINE CHEM MATERIAL FACTORY
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Problems solved by technology

[0003] Existing peptide synthesis generally adopts solid-phase or synthetic methods. On the one hand, the consumption of raw materials during synthesis is large, the synthesis equipment is expensive, the processing and synthesis efficiency is low, the purity is low, the synthesis reaction process is complicated, and it is not easy to separate; on the other hand, the synthesis The equipment used is expensive, and the production cost is high, which cannot meet the needs of small and medium-sized enterprises for processing and synthesis.

Method used

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Embodiment Construction

[0018] A kind of preparation method for 9-fluorenyl methaneoxycarbonyl succinimide of the present invention is described in detail below in conjunction with specific examples:

[0019] The invention provides a method for preparing 9-fluorenyl methaneoxycarbonyl succinimide, comprising the following steps,

[0020] Step 1, at first the mass ratio is 1:3-4 fluorenyl methaneoxycarbonyl chloride formate and succinic acid imine are dissolved in water

[0021] liquid as a raw material, then control the reaction temperature at 40°C-60°C, and slowly stir the reaction for 10m-30m to obtain the reaction liquid;

[0022] Step 2, adding an inorganic base to the reaction solution in step 1 and stirring the reaction, wherein the inorganic base is sodium carbonate or sodium bicarbonate and the mass ratio is 2-4 times that of the succinic acid immonium aqueous solution;

[0023] Step 3. Filter, wash and dry the reaction solution prepared in step 3 to obtain 9-fluorenylmethoxycarbonyl succini...

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Abstract

The invention specifically discloses a preparation method for 9-fluorenylmethoxycarbonyl succinimide, which belongs to the technical field of synthetic materials. The preparation method comprises the following steps: 1, using fluorenylmethoxycarbonyl chloroformate and an aqueous imidosuccinic acid solution in a mass ratio of 1: 3-4 as raw materials; 2, adding inorganic base in a reaction liquid obtained in step 1 and carrying out a reaction with stirring, wherein the inorganic base is sodium carbonate or sodium bicarbonate, and a mass ratio of the inorganic base to the aqueous imidosuccinic acid solution is 2 to 4; and 3, subjecting a reaction solution obtained in step 2 to filtration, washing and drying so as to obtain 9-fluorenylmethoxycarbonyl succinimide, wherein drying temperature is 30 to 80 DEG C. The preparation process provided by the invention overcomes the problems of low efficiency, low purity and a complex method in conventional processing and synthesis technology and can rapidly and easily process and synthesize 9-fluorenylmethoxycarbonyl succinimide with high purity; meanwhile, the price of equipment used in processing and synthesis is moderate, so needs of middle and small-sized enterprises for processing and synthesis are met, and investment for production cost of the enterprises is reduced.

Description

technical field [0001] The invention relates to the technical field of synthetic materials, in particular to a preparation method for 9-fluorenylmethoxycarbonyl succinimide. Background technique [0002] As we all know, 9-fluorenyl methaneoxycarbonyl succinimide is mainly used in the processing of peptide synthesis products to protect amino acids. It is an organic compound between amino acids and proteins. Through the study of the synthesis process of peptides Discovery has become one of the important research directions in the field of biochemistry. [0003] The existing peptide synthesis generally adopts solid-phase or synthetic methods. On the one hand, the consumption of raw materials is large and the synthesis equipment is expensive, the processing and synthesis efficiency is low, the purity is low, the synthesis reaction process is complicated, and it is not easy to separate; on the other hand, the synthesis The equipment used is expensive, and the production cost is ...

Claims

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Application Information

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IPC IPC(8): C07D207/46
Inventor 倪明前
Owner TAICANG HENGYI MEDICINE CHEM MATERIAL FACTORY