Electric Literature of 461-17-6, 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 461-17-6 as follows.
Example 2; 1-(2,4-Dichlorophenyl)-4-methyl-5-[4-(4,4,4-trifluorobutoxy)-phenyl]-1H-pyrazole-3- carboxylic acid piperidin-1-ylamide; 1- (2, 4-Dichlorophenyl)-5- (4-hydroxyphenyl)-4-methyl-1H-pyrazole-3-carboxylic acid piperidin-l-yl amide from Ex 1, Step F (250 mg, 0.56 mmol) was dissolved in acetone (10 ml) and potassium carbonate (77 mg, 0.56 mmol) was added followed by 1-iodo-4, 4,4- trifluorobutane (140 mg, 0.56 mmol). The reaction mixture was boiled under reflux overnight, concentrated and purified by flash chromatography (hexane : EtOAc 70: 30- 60: 40) afforded 130 mg (42%) of a white solid that was triturated with hexane: EtOAc 95 : 5 and filtered. ‘H NMR (CDC13) : 5 7.63 (1H, broad s), 7.43 (1H, m), 7.30 (2H, m), 7.10-7. 00 (2H, m), 6.85-6. 78 (2H, m), 4.05 (2H, t), 2.90 (4H, m), 2.40-2. 19 (SH, s and m), 2.15-1. 97 (2H, m), 1. 78 (4H, m), 1.45 (2 H, m) MS m/z 577 (M+Na). HPLC: 98.4%
According to the analysis of related databases, 461-17-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/80343; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com