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ChemicalBook CAS DataBase List 2,4-Dihydroxypyrimidine-5-carboxylic acid
23945-44-0

2,4-Dihydroxypyrimidine-5-carboxylic acid synthesis

9synthesis methods
Thymine

65-71-4

2,4-Dihydroxypyrimidine-5-carboxylic acid

23945-44-0

The general procedure for synthesizing uracil-5-carboxylic acid from 5-methyluracil was as follows: 100 g of 5-methyluracil and 300 mL of deionized water were added to an autoclave reactor, followed by the addition of 35 mL of a 30% hydrogen peroxide solution. Next, 15 g of 1-hydroxy-1,2,3-benzotriazin-4(3H)-one and 35 g of a pre-prepared catalyst (as described in Example 3) were added. The atmosphere in the autoclave was replaced with oxygen and the reaction system was subsequently heated to 130°C and maintained at this temperature for 3 hours. Upon completion of the reaction, the reaction solution was cooled to room temperature and filtered to remove insoluble material. The filtrate was concentrated under reduced pressure and poured into an ice-water mixture for cooling and crystallization, resulting in 150 g of white solid product. The yield of this step was 96.1%, and the purity of the product was 99.3% as analyzed by high performance liquid chromatography (HPLC).

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Yield:23945-44-0 96.1%

Reaction Conditions:

with dihydrogen peroxide;1-hydroxy-1,2,3-benzotriazine-4(3H)-one in water at 130; for 3 h;Autoclave;Temperature;

Steps:

6
Add 100 g of thymine and 300 mL of water to the autoclave, and add 35 mL of hydrogen peroxide at a concentration of 30%.15 g of 1-hydroxy-1,2,3-benzotriazine-4(3H)-one and 35 g of the catalyst prepared in Example 3, replacing the inside of the autoclave with an oxygen atmosphere, and heating to 130 ° C for 3 h.The reaction solution was cooled, filtered, concentrated, and placed in an ice-water mixture to cool.150 g of a white solid was precipitated, the yield was 96.1%, and the purity was 99.3%.

References:

Zhengzhou Gaike Technology Co., Ltd.;Guo Libing;Fan Liming CN108341785, 2018, A Location in patent:Paragraph 0014-0020

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