Related Products of 41253-21-8,Some common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE 30 Preparation of bis(4-Fluorophenyl)methyl(1H,-1,2,4-triazol-1-ylmethyl)silane and its hydrochloride salt A mixture of 4.2 g (0.015 mol) of (chloromethyl)bis(4-fluorophenyl)methylsilane and 1.4 g (0.015 mol) of 1,2,4-triazole sodium salt in 8 ml of dimethylformamide was stirred at 80 for 2 hours. The resulting slurry was cooled, diluted with water, and washed with ether. The ether extracts were washed with several portion of water and once with brine, dried over magnesium sulfate, and evaporated to leave 4.0 g of a pale yellow oil. Impurities were removed by Kugelrohr distillation at 120-125 (0.05 mm), leaving behind 2.3 g (49%) of the title compound as a yellow oil: nD21 1.5538; ir (neat) 3065, 3030, 2960, 2925, 1590, 1500, 1270, 1235, 1165, 1110, 1010, 830, 790 cm-1; nmr (CDCl3): 0.7 (3H, s), 4.2 (2H, s), 7.1 (4H, t, J=9), 7.5 (4H, d of d, J=6 and 9), 7.8 (1H, s) and 7.9 (1H, s). A sample prepared similarly was crystallized from hexane at -20 C. to give colorless solid, m.p. 52-53. The hydrochloride salt of the title compound was prepared as follows. A solution of 5.0 g (0.016 mol) of [bis(4-fluorophenyl)]methyl(1H-1,2,4-triazol-1-ylmethyl)silane in 100 ml of toluene was stirred while HCl gas was passed over the solution surface until no further precipitate formed. The colorless solid was collected by filtration, washed with toluene and petroluem ether, and air-dried to give 5.1 g (91%) of the hydrochloride salt, m.p. 195-197. Recrystallization from 100 ml of hot ethanol gave 3.5 g of colorless crystals, m.p. 201-203. Acid salts of the other triazoles of this invention can be prepared similarly. By applying the procedures of Examples 24 and 26-30 to appropriate chloromethylsilanes, the compounds of Table VI can be prepared.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Sodium 1,2,4-triazol-1-ide, its application will become more common.
Reference:
Patent; E. I. Du Pont de Nemours and Company; US4510136; (1985); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics