33252-63-0Relevant articles and documents
Novel process for synthesizing cyproconazole intermediate alpha ketone
-
Paragraph 0018, (2020/12/15)
The invention relates to a novel process for synthesizing cyproconazole intermediate alpha ketone, which comprises the steps of reacting a metered potassium hydroxide aqueous solution with 2-fluorine-5-trifluoromethylpyridine, neutralizing with sulfuric acid, filtering, washing, drying to obtain trifluoropyridinol, and reacting DMF, trifluoropyridinol, methyl o-chloromethylphenylacetate and sodiumhydroxide to obtain ether ester; then reacting toluene, ether ester, methyl formate and sodium hydroxide for desolvation to obtain enol; and finally reacting dichloromethane, enol, dimethyl sulfate and sodium hydroxide, filtering and drying to obtain a finished picoxystrobin product, so that the whole reaction condition is mild, the operation is simple, the method is a relatively ideal industrialsynthesis route, the total synthesis yield reaches 65% or above, and the product content reaches 97%.
A for the synthesis of anti-cancer auxiliary drug pyridine medical process for the preparation of intermediates
-
Paragraph 0023, (2017/01/26)
The invention relates to the field of medical chemistry and discloses a method for synthesizing a pyridine medical intermediate, namely 2-bromo-3-chloro-5-trifluoromethyl pyridine, for synthesizing anti-cancer auxiliary medicines. The method comprises the following steps of: (1) reacting 6-hydroxynicotinic acid, hydrofluoric acid and sulfur tetrafluoride at the temperature of between 100 and 120DEG C and under the pressure of 0.1-0.3MPa, and adding water to obtain 2-hydroxy-5-trifluoromethyl pyridine; (2) reacting with N-chlorosuccinimide, and performing water precipitation to obtain 3-chloro-5-trifluoromethyl-2-hydroxypyridine; and (3) adding excessive phosphorus oxybromide, reacting at the temperature of between 145 and 160DEG C for 5 to 8 hours, cooling, violently stirring at the temperature of between -5 and 0DEG C, extracting, combining organic phases, drying, filtering, performing spin drying, and purifying by using a silica gel column. According to the method, raw materials are readily available, the cost is low, the method is suitable for industrial production and the yield exceeds 38 percent.
Synthesis of the N-substituted pyridin-1(2H)-one framework by ligand-assisted Pd-catalyzed reactions
Zhou, Kang,Wen, Ping,Chen, Wenlin,Ma, Chaowei,Huang, Guosheng
, p. 448 - 452 (2013/02/25)
An efficient Pd-catalyzed method for the synthesis of N-substituted pyridin-1(2H)-ones was developed. The corresponding derivatives, which can be found in numerous biologically active compounds, were obtained in good to excellent yields. A possible mechanism for this reaction is discussed. An efficient ligand-assisted palladium-catalyzed approach for the straightforward synthesis of the pyridin-2(1H)-one framework was developed. This method provides one of the easiest pathways to access this class of valuable compounds from easily available starting materials (2-chloropyridines). A possible mechanism for this reaction is discussed. Copyright
