Electric Literature of 89570-84-3, 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. 89570-84-3, name is 2-Hydrazinyl-4-(trifluoromethyl)pyridine. A new synthetic method of this compound is introduced below.
631 mg (3.0 mmol) of the compound from Example 3A and 531 mg (3.0 mmol) of the compound from Example 25A are initially introduced into 10 ml ethanol. 114 mg (0.6 mmol) p-toluenesulfonic acid monohydrate are added and the mixture is stirred under reflux for 16 h. It is then concentrated and the residue is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% TFA). The product fractions are combined, the solvent is removed and the residue is dried under a high vacuum. 20 ml of a 4 N solution of hydrogen chloride in dioxane are added and the mixture is stirred at RT for 1 h. The solid is filtered off, washed twice with tert-butyl methyl ether and dried under a high vacuum.Yield: 231 mg (23% of th.)LC-MS (Method 8): Rt=1.65 min; MS (ESIpos): m/z=297 [M+H]+;1H-NMR (400 MHz, DMSO-d6): delta=8.81 (d, 1H), 8.70 (s, 1H), 8.59 (s, 1H), 8.47 (s, 1H), 7.92 (s, 1H), 7.77 (d, 1H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,89570-84-3, 2-Hydrazinyl-4-(trifluoromethyl)pyridine, and friends who are interested can also refer to it.
Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; US2010/305085; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem