22884-10-2, These common heterocyclic compound, 22884-10-2, name is 2-(1H-Imidazol-1-yl)acetic acid, its 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.
A mixture of 1-imidazolylacetic acid (25g; 0.1538mol) and H3PO3 (18.9g; 0.2306mol) in N,N’-dimethylethyleneurea (DMEU) (150ml) is heated to a temperature of from 4O0C to 500C. PCl3 (26ml; 0.3076mol) is slowly added to the resulting suspension. The resulting mixture is heated to a temperature of from 500C to 6O0C and stirred until reaction is complete by HPLC. Water is slowly added to the reaction mixture and the resulting solution is heated, with stirring, to a temperature of from 800C to 1000C until the reaction is complete. The reaction mixture is cooled to ambient temperature and the pH is adjusted to pH 8.0 to 9.0 with aqueous sodium hydroxide solution. The resulting solution is filtered and the pH of the solution is adjusted to pH 1.5 to 2.0. Ethanol is added and precipitation of solids occurs. The solid is filtered, washed and dried under vacuum at a temperature of from 45C to 550C to a constant weight. 25.7g of zoledronic acid is obtained (molar yield: 85.6%) with a HPLC purity higher than 99.5% in area. [The yield was calculated on dry basis]The product was characterized as follows:1H NMR (D2O) delta=4.71 (t, 2H, CH2); 7.28 (dd., IH3CH); 7.44 (dd., IH, CH); 8.62 (s., IH, CH)31P NMR (D2O) delta= 16.03
Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 22884-10-2.
Reference:
Patent; HOVIONE INTER LIMITED; TURNER, Craig, Robert; WO2008/56129; (2008); A1;,
Imidazole – Wikipedia,
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