Introduction of a new synthetic route about 1-Methyl-1H-1,2,3-triazole

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-1,2,3-triazole, and friends who are interested can also refer to it.

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 16681-65-5 name is 1-Methyl-1H-1,2,3-triazole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 16681-65-5

The title compound was prepared according to No. WO2008 / 135826 International Patent Application Publication. In 1-methyl -1H-1,2,3- triazole (1.0g, 12.0 mmol, prepared according to International Patent Application No. 2008098104) 50 mL 2-neck flask containing, by the addition of THF (45 mL) , colorless solution was cooled to -40 . Then, by adding dropwise the (2.5 M, 4.8 mL, 12.0 mmol in hexane) n-BuLi, to give a dark reddish brown viscous solution. The mixture was stirred for 45 minutes at -30 to -20 in the following, was introduced into a pure DMF (3mL, 38.5 mmol) at -10 . The mixture was allowed to warm to room temperature, after stirring for 60 minutes, poured into water. Extract the aqueous portion with EtOAc (4 ¡Á 50 mL), the combined organics washed with brine, dried with MgSO4, filtered, and concentrated. The aqueous portion was extracted with DCM (3 ¡Á 50 mL) station, and dried as described above. The combined organics were concentrated to give a light brown oil The UV activity much higher than the starting material. DCM-25% CH3CN, according to TLC or of from 25% EtOAc-DCM, showed the product has a slightly higher Rf than the starting material. (With 100% DCM, 25% CH3CN-DCM increased) by silica gel chromatography on to give the title compound as a colorless oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-1,2,3-triazole, and friends who are interested can also refer to it.

Reference:
Patent; Janssen Pharmaceuticals N.V; Leonardo, Christi.A.; Barvei, Kent; Edward, James P.; Gloita, Kevin D.; Kummer, David .A.; Maharoof, Umar; Nishimura, Rachael; Urbanski, Mode; Venkatesan, Hariharan; Wang, Ai Hua; Olin, Ronald L.; Woods, Craig; Fourier, Anne; Shu, Jih; Cumings, Maxwell D.; (86 pag.)KR2016/68948; (2016); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics