Preparation method for o-chlorobenzonitrile
A technology of o-chlorobenzonitrile and o-chlorobenzoic acid, which is applied in the preparation of organic compounds, the preparation of carboxylic acid amides, chemical instruments and methods, etc., can solve the problem that o-chlorobenzaldehyde oxime is expensive, affects yield and product quality, The effect is not very ideal, and the effect of avoiding complex process equipment, stable product quality and less pollution can be achieved.
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Embodiment 1
[0038] In the 500ml four-neck flask that thermometer and distillation column are housed, add 160 g content and be the o-chlorobenzoic acid of 98.0%, the urea of the massfraction 46.3% of 61g total nitrogen (N) amount, open heating mantle power supply to heat up, when
[0039] When the temperature rises to 145°C, the melting is almost complete, and the stirring is turned on. The early stage reaction is controlled at 140-180°C, and the reaction lasts for 4 hours. The molar ratio of o-chlorobenzoic acid to urea is 1:1. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography to be 81.2%. The ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.
[0040] Slowly heat up, the temperature reacts at 230~250°C for 1.5 h, then continues to heat up and controls at 250~270°C, reacts for 1.5h, distills out the crude nitrile under reduced pressure, and the residue aft...
Embodiment 2
[0044] In the 500ml four-necked flask that thermometer and distillation column are housed, add 160 g content and be the o-chlorobenzoic acid of 98.0%, the urea of the massfraction 46.0% of 85g total nitrogen (N) amount, open heating mantle power supply to heat up, when When the temperature rises to 145°C, the melting is almost complete, and the stirring is turned on. The early stage reaction is controlled at 140-180°C, and the reaction lasts for 4 hours. The molar ratio of o-chlorobenzoic acid to urea is 1:1.4. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography to be 89.1%. The ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.
[0045] Slowly heat up, the temperature reacts at 230~250°C for 1.5 h, then continues to heat up and controls at 250~270°C, reacts for 1.5h, distills out the crude nitrile under reduced pressure, and the residue after dist...
Embodiment 3
[0049] In the 500ml four-neck flask that thermometer and distillation column are housed, add 160 g content and be the o-chlorobenzoic acid of 98.0%, the urea of the massfraction 46.4% of the total nitrogen (N) amount of 85g, open heating mantle power supply and heat up, when The temperature rose to 145°C and basically melted, and the stirring was turned on, the reaction temperature was controlled at 140-180°C, and the reaction was carried out for 2 hours. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography to be 88.3%. The ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.
[0050] Slowly heat up, the temperature is reacted at 230-250°C for 4 h, then continue to heat up and control at 250-270°C, react for 3h, distill the crude nitrile under reduced pressure, the residue after distillation contains the intermediate produced by the reaction, and sta...
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