1157938-97-0, name is 1-(2,5-Difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone, belongs to Triazoles compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of 1-(2,5-Difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone
Indium powder (15.4 g, 133.8 mmol) was dissolved in dry THF (150 mL).Replace with nitrogen three times, then cool to 0C and slowly add(S)-2-Bromo-propionitrile (8,90,66.9 mmol) stirring for 30 min,Then slowly adding 1-(2,5-difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone dissolved in(9.95 g, 44.6 mmol) of dry THF (15 mL) was stirred at -10C for 10 hours,Until the disappearance of raw materials, filtration, the filtrate was added 200mL of n-hexane stirring for 40min,Cool, filter, wash with water, and dry to obtain (2S, 3R) andA mixture of (2R, 3S) 11.1 g, (yield 89.5%, d.e. > 99.2%).The resulting white solid was dissolved in 20 ml of toluene, 40 ml of methyl tert-butyl ether andIn a mixed solvent of 10 mL methanol,Add D-10-camphorsulfonic acid (7.09 g, 30.56 mmol) to heat the reaction to 60C,After reacting for 1 h, slowly cooling and cooling, filtering to obtain a white solid, then adding water,Stir with sodium bicarbonate and extract with dichloromethane.The organic phase was concentrated to obtain 9.4 g of the (2S,3R) diastereoisomer according to Formula (I).(Yield: 84.7%, e.e. > 99.1%, d.e. > 99.2%).The results of the LC-MS and H-NMR measurements of the resulting compound were the same as those described in Example 2.
The synthetic route of 1157938-97-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Liu Meijun; (18 pag.)CN106317044; (2017); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics