2-chloro-3-cyanopyridine preparation process
A cyanopyridine and preparation technology, which is applied in the field of the preparation of intermediates in the chemical industry, can solve the problems of increasing the difficulty of enterprise wastewater treatment, environmental hazards, etc., and achieve the effect of good yield and increased yield
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Embodiment 1
[0017] Weigh 50g of chloroform and add it to a 250ml three-necked flask, weigh 10g of N-oxonicotinic acid amide and add it to the three-necked flask, cool down to 15±5°C, weigh 20g of phosphorus oxychloride and add it dropwise to the three-necked flask with a controlled dropping time of 1.5h In the flask, after the dropwise addition is completed, then cool down to 10±5°C, weigh 10g of triethylamine and 1g of tri-n-propylamine and mix them evenly, and drop them into the three-necked flask at a controlled dropping time of 0.5h. After the dropwise addition, keep the temperature at Continue to stir at 5°C for 20 minutes, heat up to 25°C, keep stirring for 30 minutes, then raise the temperature to 50°C, keep stirring for 30 minutes, then raise the temperature to 95°C, keep stirring for 3 hours, and obtain the chloride reaction solution after the heat preservation, transfer the chloride reaction solution In the rotary evaporator, control the temperature at 50°C and the pressure at 2K...
Embodiment 2
[0019] Weigh 80g of dichloromethane and add it to a 250ml three-necked flask, weigh 10g of N-oxonicotinamide and add it to the three-necked flask, cool down to 15±5°C, weigh 30g of phosphorus oxychloride and add it dropwise to In the three-necked flask, after the dropwise addition is completed, cool down to 10±5°C, weigh 8g of diethylamine and 5g of di-n-propylamine and mix them evenly, and drop them into the three-necked flask for 1 hour. After the dropwise addition, keep the temperature at Continue to stir at 10°C for 30min, heat up to 35°C, keep stirring for 1h, then raise the temperature to 55°C, keep stirring for 1h, then raise the temperature to 97°C, keep stirring for 4h, after the heat preservation is completed, the chloride reaction solution is obtained, and the chloride reaction solution is transferred In the rotary evaporator, control the temperature at 60°C and the pressure at 5Kpa for rotary evaporation, until no obvious liquid flows out, measure 40ml of water into...
Embodiment 3
[0021] Weigh 100g of dichloroethane and add it to a 250ml three-necked flask, weigh 10g of N-oxonicotinamide and add it to the three-necked flask, cool down to 15±5°C, weigh 40g of phosphorus oxychloride and control the dropping time to 2.5h. Add it into the three-necked flask, after the dropwise addition is completed, then lower the temperature to 10±5°C, weigh 7g of triethylamine and 8g of n-butylamine and mix them evenly, control the dropping time for 1.5h and drop them into the three-necked flask, after the dropwise addition is completed, Keep the temperature at 15°C and continue to stir for 40min, then raise the temperature to 45°C, keep stirring for 1.5h, then raise the temperature to 60°C, keep stirring for 1.5h, then raise the temperature to 100°C, keep stirring for 5h, and obtain the chloride reaction solution after the heat preservation is completed. Transfer the chloride reaction liquid to a rotary evaporator, control the temperature at 70°C, and carry out rotary eva...
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