Preparation method of 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid
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A cyclic acid and fumaric acid technology, applied in the direction of organic chemistry, can solve problems such as control difficulties, and achieve the effects of optimizing reaction temperature, short synthesis route and improving product yield
Active Publication Date: 2017-06-13
安徽泰格维生素实业有限公司
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[0006] The solvent ratio and reaction concept of the traditional cyclic acid process are relatively conservative, and the control is relatively difficult
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Embodiment 1
[0045] A preparation method of cyclic acid, comprising the following steps:
[0046] 1) The addition reaction of bromination generates dibromosuccinic acid adduct:
[0047] Add 60g of fumaric acid, 70g of water, and 12g of concentrated hydrobromic acid (5.5% by mass) into the reaction flask, raise the temperature to 60-70°C, add 80g of bromine dropwise, keep a certain pressure in the reaction flask, and raise the temperature to 70 ~90°C, keep warm for 5-10 hours, cool down, crystallize, and filter to obtain compound I (ie, dibromosuccinic acid adduct).
[0048] 2) Amination substitution reaction to generate dibenzylamide potassium salt
[0049]Put 60g of compound I (dibromosuccinic acid adduct) and 250ml of amination mother liquor into the reaction flask, control the temperature at 20-50°C, add 129g of benzylamine dropwise, and control the temperature at 20-50°C during the dropping process, Raise the temperature to 70-90°C, keep it warm for 5-10 hours, cool down, filter, add...
Embodiment 2
[0053] A preparation method of cyclic acid, the only difference from Example 1 is: step 2) the amination substitution reaction uses about 250ml of the amination mother liquor produced in the previous batch; the obtained dibenzylamide potassium salt HPLC content is 99.5%, and the yield The rate is 85%.
Embodiment 3
[0055] A preparation method of cyclic acid, the difference from Example 1 is only: step 1) adopts mass fraction 5.5% hydrobromic acid to stabilize the reaction concentration in the bromination addition reaction; the prepared dibromosuccinic acid HPLC content is 99% %, the yield is 93%.
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Abstract
The invention relates to a preparation method of 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid, comprising the steps of subjecting fumaric acid, bromine and hydrobromic acid to additive reaction to generate meso-2,3-dDibromosuccinic acid, subjecting the meso-2,3-dDibromosuccinic acid, benzylamine and a strong base to aminating reaction to generate dibenzylamino salt, subjecting the dibenzylamino salt and triphosgene to cyclization to generate the 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid. The fumaric acid is subjected to addition, and then substitution and cyclization are performed to obtain the 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid, and detection shows that HPLC (high-performance liquid chromatography) content of the 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid may reach 98-99%. The preparation method has the advantages that hydrobromic acid is added for bromination additive reaction, the concentration and reaction temperature of the hydrobromic acid are optimized, and bromine loss is more reduced; amination mother liquid is used in amination, the cost is saved, and product yield is increased; in ring-closure reaction, pH and reaction product concentration are decreased, the yield of the 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid is increased greatly, and the quality of the 1,3-dibenzyl-2-oxoimidazolidine-4,5-dicarboxylic acid is improved; experiments verify that through process innovation, production cost is reduced greatly, production efficiency is improved, and the process is energy efficient and environmentally friendly.
Description
technical field [0001] The invention belongs to the technical field of preparation of vitamin H raw materials, and in particular relates to a preparation method of cyclic acid. Background technique [0002] The structural formula of cyclic acid is shown below, and its CAS number is 59564-78-2. [0003] [0004] Cyclomic acid is an essential and main raw material for the production of biotin, namely vitamin H, by the new process. Biotin is one of the B vitamins, also known as vitamin H, vitamin B7, and coenzyme R (Coenzyme R). It is a factor that can prevent hair loss and skin damage in rats induced by feeding raw egg protein from the liver when studying yeast growth factors and rhizobia growth and respiration promoting factors in the 1930s. Biotin is a member of the water-soluble vitamin B group. It is more abundant in liver, kidney, yeast, and milk, and is an important factor for organisms to fix carbon dioxide. It is a necessary substance for the synthesis of vitamin...
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