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1 results about "Oxalyl chloride" patented technology

Oxalyl chloride is a chemical compound with the formula (COCl)₂. This colourless, sharp-smelling liquid, the diacyl chloride of oxalic acid, is a useful reagent in organic synthesis. It can be prepared by treating oxalic acid with phosphorus pentachloride.

Method for preparing N,N-diethyl-3-pyridine carboxamide

InactiveCN104387319AHigh boiling pointLow boiling pointOrganic chemistryDistillationSynthesis methods
The invention discloses a method for preparing N,N-diethyl-3-pyridine carboxamide. The method comprises the following steps: adding nicotinic acid and dichloromethane into a reaction bottle and dropwise adding oxalyl chloride at the temperature of 0 DEG C; after oxalyl chloride is added dropwise, stirring and reacting at the temperature of 0 DEG C for 0.5-1 hour and reacting at room temperature for 4-6 hours; after the reaction is ended, dropwise adding a sodium hydroxide solution for regulating the pH value of the reaction solution to 7, slowly dropwise adding diethylamine at the temperature of 5 DEG C below zero to 10 DEG C; after diethylamine is added dropwise, reacting at the room temperature for 6-8 hours; after the reaction is finished, adding a sodium carbonate solution, stirring, standing for layering, removing the lower water layer, drying the organic layer, thereby obtaining a crude product of N,N-diethyl-3-pyridine carboxamide; adding the crude product of N,N-diethyl-3-pyridine carboxamide into dichloromethane, discoloring, oxidizing, removing dichloromethane, performing reduced-pressure distillation, thereby obtaining the finished product of N,N-diethyl-3-pyridine carboxamide. The method is low in equipment requirement, slight in environmental pollution and low in danger coefficient and is a synthesis method which is environment-friendly and very suitable for industrial production.
Owner:HENAN LINGXIAN SCI & TECHN PHARMA
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