Application of 4928-88-5,Some common heterocyclic compound, 4928-88-5, name is Methyl 1H-1,2,4-triazole-3-carboxylate, molecular formula is C4H5N3O2, 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.
In a 6000 ml 4-necked anhydrous reactor equipped with a thermometer, a condenser and a mechanical stirrer, 1680 ml of dichloromethane, 400.05 g of tetraacetyl ribose and 185.11 g of 3-carbomethoxytriazole were added while stirring and introducing nitrogen. The mixture was cooled to about 5 ¡ã C and 360.03 g of tin tetrachloride was added to the suspension as a trickle while stirring, and the reaction was allowed to exotherm by cooling with an ice bath so that the temperature did not exceed 15-20 ¡ãC, and when fully added, the reaction mixture was heated to reflux for 2 h, cooled to 20 ¡ã C with water and ice bath over 15 min.Then 30percent hydrochloric acid (176.7 ml) and water (1503.3 ml) were added at a temperature below +20 ¡ã C and stirred for 45 min; the mixture was allowed to stand for 15 min to separate, and then the aqueous phase of the upper layer was separated from the enriched organic phase, followed by The organic phase was treated with 30percent hydrochloric acid (176.7 ml) and water (1503.3 ml).After stirring for 45 min, the mixture was allowed to stand for 15 min to separate the phases, the upper aqueous phase was separated from the enriched organic phase, and then the organic phase was treated with 30percent hydrochloric acid (176.7 ml) and water (1503.3 ml). After 45 minutes,The mixture was allowed to stand for 15 min to separate the phases by phase separation: the organic phase was distilled at atmospheric pressure (internal temperature 45 ¡ã C) and 3000 ml of toluene was added to the oil residue, and the mixture was distilled under vacuum at a residual pressure of about 200 mbar. Stirred moist paste.It was allowed to cool to 5-10 ¡ã C for 2 h and was filtered on a Buchner funnel while washing with toluene. 521.36 g of a moist product were obtained.
The synthetic route of 4928-88-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Li Shuangxi; (12 pag.)CN109134565; (2019); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics