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. 6818-99-1, name is 3-Chloro-1,2,4-triazole, A new synthetic method of this compound is introduced below., Quality Control of 3-Chloro-1,2,4-triazole
A mixture of 3-chloro-lH-l,2,4-triazole (2.76 g, 26.7 mmol), 1- chloro-2-methoxy-4 -nitrobenzene (5.0 g, 26.7 mmol), potassium hydroxide flakes (1.496 g, 26.7 mmol), and DMSO (25 mL) was heated in a sealed reaction vessel 100 0C for 24 h. The reaction was allowed to cool to rt and additional portions of 3- chloro-lH-l,2,4-triazole (1.38 g, 0.5 equiv) and potassium hydroxide (0.75 g, 0.5 equiv) were added. The reaction vessel was resealed and heated to 1100C for an additional 24 h. The resulting mixture was allowed to cool to rt and was poured into 500 mL of water. The aqueous mixture was extracted with EtOAc (3 x 100 mL). The combined organics were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude residue was purified using silica gel chromatography (0-5% MeOH/chloroform, linear gradient over 144 min, flow 25 mL/min) to afford 2-(3-chloro-lH-l,2>;4-triazol-l-yl)-5-nittophenol (0.924 g, 3.84 mmol, 14.4 % yield). LC-MS (M+H)+ – 241.0. 1H NMR (500 MHz, chloroform-^ delta ppm 11.97 (br. s., 1 H) 9.24 (s, 1 H) 7.90 – 7.95 (m, 1 H) 7.89 (d, J=2.44 Hz, 1 H) 7.84 (dd, J=8.85, 2.44 Hz, 1 H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; MARCIN, Lawrence, R.; THOMPSON, Lorin, A., III; BOY, Kenneth, M.; GUERNON, Jason, M.; HIGGINS, Mendi, A.; SHI, Jianliang; WU, Yong-Jin; ZHANG, Yunhui; MACOR, John, E.; WO2010/83141; (2010); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics