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. 151899-62-6, name is 3-Iodo-1-trityl-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., Quality Control of 3-Iodo-1-trityl-1H-1,2,4-triazole
Nitrogen gas was bubbled through a solution of 3-iodo-l-trityl-lH-l,2,4-triazole (37.3g, 85.35mmol), and triethylamine (17.8ml, 128mmol) in anhydrous DMF (300ml) heated at 350C for 30 mins. Pd(PPh3)2Cl2 (2Ag, 3.4mmol) and CuI (651mg, 3.4mmol) were added followed by addition of ethynyltrimethylsilane (18ml, 128mmol) in anhydrous DMF (18ml) over 5 15 hours via syringe pump. After complete addition the mixture was heated at 350C for a further 5 hours. The mixture was poured into water (700ml) and extracted with EtOAc (3 x 300ml). Combined EtOAc layers washed with water (2 x 500ml), sat. NaCl (250ml), dried over Na2SO4, filtered and evaporated. The residue was purified by MPLC on silica gel eluting with a gradient from 100% hexanes to 10% EtOAc in hexanes to afford the title compound. 1HNMR (500 MHz, 10 CDCl3) delta: 7.96 (s, IH), 7.37 (m, 9H), 7.14 (m, 6H), 0.27 (s, 9H).
The synthetic route of 151899-62-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK & CO., INC.; WO2008/57336; (2008); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics