Sep 2021 News Analyzing the synthesis route of 5305-59-9

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5305-59-9, 6-Chloropyrimidin-4-amine, and friends who are interested can also refer to it.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.5305-59-9, name is 6-Chloropyrimidin-4-amine, molecular formula is C4H4ClN3, molecular weight is 129.55, as common compound, the synthetic route is as follows.Application In Synthesis of 6-Chloropyrimidin-4-amine

Step 1: Take a dry three-mouth reaction bottle and place the magnet.Add 4-amino-6-chloropyrimidine (1 eq), KI (0.5 eq),It was dissolved in absolute ethanol (35 mL).After stirring for 10 min on a magnetic stirrer,Trifluoroacetic acid (200 mL) was added. activation.After about 1 h, a solution of the substituted aniline (0.8 eq) dissolved in absolute ethanol (15 mL) was added.Note that you have to add it by drop,In order to achieve long-term excess reaction,The dropping time is controlled at around 1h. Step 2: The progress of the reaction and the reaction effect were examined by the TLC method.Generally, after 36 hours of reaction, the reaction is almost complete.After the reaction is completed, the solvent is dried in absolute ethanol.Then a certain amount of ethyl acetate was added to dissolve.First remove the acid with an appropriate amount of 20% sodium bicarbonate solution.Then add a certain amount of 50% sodium chloride solution to extract the layering.Collect the organic layer and spin it to a certain amount.Add an appropriate amount of anhydrous sodium sulfate and remove water overnight. Step 3: suction filtration, sand making,Weigh 15 to 20 times the total amount of raw materials and install the column silica gel powder column, and collect the product points through the column.Generally use petroleum ether: ethyl acetate = 2:1 to pass the first point (aniline point),Petroleum ether: ethyl acetate = 1:1 over the second point (pyrimidine point),Ethyl acetate or methanol is washed out of the product.The spin-dried product points were collected, dried in an oven, mass spectrometrically and nuclear magnetically verified.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5305-59-9, 6-Chloropyrimidin-4-amine, and friends who are interested can also refer to it.

Reference:
Patent; Wenzhou Medical University; Ye Faqing; Cheng Donghua; Han Chao; Pan Suwei; Pan Yaqian; Xie Zixin; (14 pag.)CN109053593; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia