Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1533519-84-4, name is 4-(4-Cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione, A new synthetic method of this compound is introduced below., HPLC of Formula: C15H13N3S
Acetonitrile 600g is first added to a 1L four-neck flask at room temperature.Compound IV (106.9 g, 0.4 mol) was added with stirring.Compound Vc (57.9 g, 0.22 mol) was added. Slowly warm up to 50-55C under nitrogen protection.The solid was completely dissolved and 48g of potassium bicarbonate was added portionwise over 60-80 minutes.After the addition, the reaction was incubated at 50-55C for 3-4 hours. The disappearance of the raw material at TLC indicated that the reaction was complete.After the reaction was completed, insoluble material was removed by hot filtration, and the resulting filtrate was slowly cooled to -5C.A large number of white solids precipitated, and 50 ml of deionized water was added dropwise to the reaction flask over 1-2 hours to crystallize sufficiently.And remove inorganic salts. After deionized water is added, it is crystallized at -5C for 2 hours and filtered.The filter cake was washed with 100 ml of 95% glacial acetonitrile. The resulting compound (IIIc) was vacuum-dried,Dry at a temperature of 50-55C for 24 hours. 120.3 g of compound (IIIc) was obtained with a yield of 83%.
The synthetic route of 1533519-84-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Zhejiang Xin Donggang Pharmaceutical Co., Ltd.; Yan Jianbo; Ma Liangxiu; Lin Yi; Hong Huabin; (16 pag.)CN107739344; (2018); A;,
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