Preparation method of 4,6-dihydroxypyrimidine
The technology of dihydroxypyrimidine and hydroxypyrimidine sodium salt is applied in the field of preparation of 4,6-dihydroxypyrimidine, which can solve the problems of large environmental protection pressure, increased waste water treatment cost and high cost, and achieves reduction of environmental protection pressure and acid consumption. effect of reducing salt content
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[0018] The invention provides a kind of preparation method of 4,6-dihydroxypyrimidine, comprising the following steps:
[0019] A) providing a 4,6-dihydroxypyrimidine reaction solution, using a bipolar membrane to treat the 4,6-dihydroxypyrimidine reaction solution to obtain a bipolar membrane treatment solution;
[0020] B) Acidifying the bipolar membrane treatment solution to obtain 4,6-dihydroxypyrimidine.
[0021] In the preparation method of 4,6-dihydroxypyrimidine provided by the present invention, before acidifying the 4,6-dihydroxypyrimidine reaction solution, a bipolar membrane is used for treatment in advance, which can reduce the amount of waste water and the salt content of waste water, and acidify It can significantly reduce the acid consumption, greatly reducing the cost and environmental protection pressure.
[0022] According to the present invention, a 4,6-dihydroxypyrimidine reaction solution is first provided, and a bipolar membrane is used to treat the 4,6...
Embodiment 1
[0038]Mix 80.0g dimethyl malonate and 60.0g formamide, add excess sodium methoxide methanol solution at 100°C, keep warm for 1h after adding, to obtain 4,6-dihydroxypyrimidine sodium salt mixture; then cool down to 70°C Concentrate the methanol and add water to continue the concentration; then add water to dissolve the 4,6-dihydroxypyrimidine sodium salt mixture to form a 4,6-dihydroxypyrimidine reaction solution. Utilize bipolar membrane to it process, until the pH of bipolar membrane treatment solution is 9.0; Under 40 ℃, be 37% hydrochloric acid to gained bipolar membrane treatment solution acidification with 131.9g mass concentration, be 2.5 to solution pH, then The resulting acidified solution was suction-filtered and dried to obtain 55.9 g of 4,6-dihydroxypyrimidine product. After testing, the purity of the obtained product was 98.2%, and the yield was 82.1%.
Embodiment 2
[0040] Mix 83.9g dimethyl malonate and 62.9g formamide, add excess sodium methoxide methanol solution at 95°C, keep warm for 1h after adding, to obtain 4,6-dihydroxypyrimidine sodium salt mixture; then cool down to 70°C Concentrate the methanol and add water to continue the concentration; then add water to dissolve the 4,6-dihydroxypyrimidine sodium salt mixture to form a 4,6-dihydroxypyrimidine reaction solution. Utilize bipolar membrane to it process, until the pH of bipolar membrane treatment solution is 10; Under 35 ℃, be 37% hydrochloric acid to gained bipolar membrane treatment solution acidification with 119.2g mass concentration, be 2.8 to solution pH, then The resulting acidified solution was suction filtered and dried to obtain 59.0 g of 4,6-dihydroxypyrimidine product. After testing, the obtained product has a purity of 98.5% and a yield of 82.5%.
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