Terbutylazine synthesis

Yield:-

Reaction Conditions:

with sodium hydroxide in water at 30 - 60;

Steps:

3.5-3.8
(6) Two-stage reactor 12 (reactor volume 5m3) The reaction liquid is pumped into the heat exchanger 13 (the material outlet temperature is controlled at 30-35 ° C) for extracorporeal circulation (circulation flow rate 25 m3 / hour) while discharging (flow rate is The two-stage reactor 12 is maintained at the same level) and enters the mixer 14, and is thoroughly mixed with the precisely metered NaOH in the mixer 4 into the second-stage neutralization tank 15, the concentration of NaOH is 30%, and the flow rate is 723 kg/hour.(7) The second stage neutralization tank 15 (reactor volume 5 m3) is pumped into the heat exchanger 16 (the material outlet temperature is controlled at 55-60 ° C) for extracorporeal circulation while discharging into the continuous stratifier 17.(8) After the oil phase partially discharged from the continuous stratifier 17 is accurately metered by the pump (the flow rate is maintained to maintain the level of the stratifier), the oil is removed into the desolvent kettle 18, and the solvent is removed by steam distillation in the desolvent kettle. The product can be obtained by performing the subsequent separation and drying.The aqueous phase from the lower part of the continuous stratifier is sent to the wastewater treatment.Through the above process, the product of Tedingjin is 1.231 tons/hour, the content is 99.2%, and the yield is 99.1%.

References:

Shandong Normal University;Chen Dongmei;Zhang Jine;Bi Yanying CN109627225, 2019, A Location in patent:Paragraph 0110; 0115-0119

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