1H-PYRAZOLE-3-CARBONITRILE synthesis

Yield:36650-74-5 85%

Reaction Conditions:

at 335; for 1 h;Temperature;

Steps:

A Nitrile Product Preparation Example A
General procedure: Following the amide intermediate Preparation Example A. The reaction vessel is closed (when the amide intermediate has a boiling point at normal pressure equal to or lower than the reaction temperature TB described below) or the reaction vessel is kept open (when the amide intermediate has a boiling point higher than the normal pressure When the reaction temperature is TB), the stirring is continued (600 r/min), the reaction temperature is changed to TB, and after the reaction temperature TB is maintained for TD hours, the reaction is almost complete. Then, the reaction vessel was sealed and connected to a vacuum pump so that the degree of vacuum in the reaction vessel reached 20-50 mbar (according to the type of nitrile product) and the distillate was used as the nitrile product. The yield of the nitrile product was calculated and sampled for nuclear magnetic proteomics and elemental analysis to characterize the nitrile product obtained. Specific reaction conditions and characterization results are shown in Tables A-7, A-8, A-9, A-10 and A-11 below. These characterization results show that the nitrile product obtained has an extremely high purity (above 99%).In these nitrile product preparation examples, 10 g of diphosphorus pentoxide was optionally added to the reaction vessel as a catalyst at the start of the reaction.

References:

Sinopec Yangzi Petrochemical Co., Ltd.;Sinopec Corporation;Sun Hailong;Wei Yanyu;Gao Yilong;Chen Xinhua;Miao Jun;Li Na;Kan Lin;Bai Jiye;Chen Shaohui;Yang Aiwu;Xu Yuexing CN104557357, 2018, B Location in patent:Paragraph 0150; 0151; 0152; 0160

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