Preparation method for orotic acid
A technology of orotic acid and acetic acid, applied in the direction of organic chemistry, can solve the problems of high process cost and limited application of orotic acid
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Embodiment 1
[0035] The invention provides a kind of preparation method of orotic acid, the preparation method of this orotic acid comprises the following steps:
[0036] (1) Synthesis of carbamoylaspartic acid: add 13.3 g of aspartic acid in the reaction vessel, then add 7 g of sodium cyanate, then add 39.9 ml of water, react at 60 ° C for 3 hours, add mass after natural cooling The concentration is 38% concentrated hydrochloric acid to pH 2.2, carbamoylaspartic acid is precipitated, the filter residue is obtained by filtration, and the filter residue is dried at 80-100°C to obtain 11 g of carbamoylaspartic acid, with a yield of 70% ;
[0037] (2) Synthesis of hydantoin acetic acid: in a reaction vessel, add 11 g of carbamoylaspartic acid, add 32 milliliters of 20 wt % hydrochloric acid, heat and evaporate to dryness, recrystallize the residue in water, and filter to obtain a filter residue , dried to obtain hydantoin acetic acid 10g, yield 81%;
[0038] (3) Synthesis of carboxymethylhy...
Embodiment 2
[0041] The invention provides a kind of preparation method of orotic acid, and its concrete steps are as follows:
[0042](1) Synthesis of carbamoylaspartic acid: add 26.6 g of aspartic acid in the reaction vessel, then add 14 g of sodium cyanate, then add 79.8 ml of water, react at 70 ° C for 4 hours, add mass after natural cooling The fraction is 38% concentrated hydrochloric acid to pH 2.3, carbamoylaspartic acid is precipitated, the filter residue is obtained by filtration, and the filter residue is dried at 80-100° C. to obtain 20 g of the product with a yield of 69%.
[0043] (2) Synthesis of hydantoin acetic acid: in a reaction vessel, add 20 g of carbamoylaspartic acid, add 60 milliliters of 20 wt % hydrochloric acid, heat and evaporate to dryness, recrystallize the residue in water, and filter to obtain a filter residue , drying the filter residue to obtain 18 g of hydantoin acetic acid with a yield of 79%.
[0044] (3) Synthesis of carboxymethylhydantoin: In a react...
Embodiment 3
[0047] The preparation method of orotic acid, its concrete steps are as follows:
[0048] (1) Synthesis of carbamoylaspartic acid: Add 39.9 g of aspartic acid in the reaction vessel, then add 21 g of sodium cyanate, then add 119.7 ml of water, react at 75 ° C for 4.5 hours, add mass after natural cooling The fraction is 38% concentrated hydrochloric acid until the pH is 2.3, and carbamoylaspartic acid is precipitated, filtered, and dried to obtain 28.5 g of the product, with a yield of 65%.
[0049] (2) Synthesis of hydantoin acetic acid: in a reaction vessel, add 28.5 g of carbamoylaspartic acid, add 85 milliliters of 20 wt% hydrochloric acid, heat and evaporate to dryness, recrystallize the residue in water, and filter to obtain The filter residue was dried to obtain 22.8 g of hydantoin acetic acid with a yield of 76%.
[0050] (3) Synthesis of carboxymethylhydantoin: In a reaction vessel, add 22.8 g of hydantoin acetic acid, then add 11.4 mL of liquid bromine, then add 45....
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