According to the analysis of related databases, 25016-11-9, the application of this compound in the production field has become more and more popular.
Application of 25016-11-9, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 25016-11-9 as follows.
Potassium terf-butoxide (23.47 g of 95%, 199.1 mmol, 2.44 equiv.) was suspended in anhydrous DME (90 mL) and cooled to – 60 0C. TosMIC (23.76 g, 121.7 mmol, 1.49 equiv.) was dissolved in anhydrous DME (75 mL), and this was added drop-wise to the potassium terf-butoxide solution over 20 minutes. After stirring for 20 minutes between – 60 and – 55 0C, the compound of formula IX, in anhydrous DME (55 ml_), was added over 23 minutes. The reaction was stirred one hour at – 55 to – 50 0C to yield a thick suspension. Methanol (90 ml_) was then added resulting in a clear brown solution. The cooling bath was removed, and after stirring 5 minutes in air, the reaction flask was immersed in an oil bath preheated to 85 0C. The reaction was stirred for 1 hour. After cooling, the mixture was concentrated and the resulting tan solid was dissolved in water (180 ml_) with acetic acid (9 ml_). This was extracted with ethyl acetate (3 x 250 ml_), and these extracts were combined, washed with saturated aqueous sodium chloride (100 ml_), dried over sodium sulfate, filtered and concentrated to yield a brown oil (13.71 g). This oil was dissolved in dichloromethane and purified by silica-gel chromatography using a gradient from 0% to 15% dichloromethane-acetone to yield the compound of formula Xl as a bright yellow oil (7.89 g, 63% yield).
According to the analysis of related databases, 25016-11-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; SCHERING CORPORATION; WO2008/153870; (2008); A1;,
Pyrazole – Wikipedia,
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