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ChemicalBook CAS DataBase List 4,6-Dichloro-5-nitropyrimidine
4316-93-2

4,6-Dichloro-5-nitropyrimidine synthesis

6synthesis methods
4,6-Dichloro-5-nitropyrimidine can be used as a pharmaceutical intermediate for the synthesis of vitamin B4. It can be obtained by the reaction of 4,6-dihydroxy-5-nitropyrimidine with phosphorus oxychloride.
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Yield:4316-93-2 97%

Reaction Conditions:

with N-ethyl-N,N-diisopropylamine;trichlorophosphate at 6 - 100; for 5 h;Temperature;Reagent/catalyst;

Steps:

1.1-4.1 Example 2: A method for synthesizing 4,5,6-triaminopyrimidine. The method for synthesizing 4,5,6-triaminopyrimidine includes the following synthesis steps:
1) Disperse 500 g of 5-nitro-4,6-dihydroxypyrimidine in 2000 ml of phosphorus oxychloride,Cool to 6 ° C and add 2,000 ml of diisopropylethylamine dropwise.A lot of white smoke is generated and the temperature rises obviously. After the addition of diisopropylethylamine is completed, the temperature is raised to 100 ° C and the reaction is performed for 5 hours.The mixture was cooled at 25 ° C and concentrated under reduced pressure to remove excess phosphorus oxychloride.The reaction was slowly poured into 5 kg of crushed ice and stirred for about 1 hour, and extracted with 2000 ml of ethyl acetate.Adjust the pH to neutral with a saturated sodium bicarbonate aqueous solution, and wash it once with a saturated sodium chloride aqueous solution.It was then dried over anhydrous sodium sulfate and concentrated to give 600 g of intermediate 6,4-dichloro-5-nitropyrimidine., Purity is greater than 98%, yield is 97%;

References:

Nanjing Puruida Pharmaceutical Technology Co., Ltd.;Wang Xiaobo CN110407757, 2019, A Location in patent:Paragraph 0022-0024; 0027-0029; 0032-0034; 0037-0039

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