AMINOPYRALID synthesis

Yield:150114-71-9 91.4%

Reaction Conditions:

with 5%-palladium/activated carbon;hydrogen;sodium hydroxide in water at 50; under 1500.15 - 2250.23 Torr; for 20 h;Reagent/catalyst;Pressure;Temperature;

Steps:

1
The 50.8 g 4-amino -3, 5, 6-trichloropyridine carboxylic acid, 500 ml water, evenly mixing 66.7 g 30% sodium hydroxide, filtering, the filtrate, is poured into the plate is provided with a magnetic stirring, thermometer, of the vent pipe 1000 ml high-pressure reaction kettle;added to the reaction kettle of 2 g 5%Pd/C , the closed reaction kettle, the replacement with nitrogen 3 times, hydrogen gas, so that the pressure to reach 0.2 MPa, stirred, the temperature is increased to 50 °C, to continue to access the hydrogen, the reaction kettle to the pressure of 0.3 MPa reaction after 20 hours, HPLC detection reaction is complete, cooling to room temperature, the reaction solution;step (2) pouring a reaction liquid, filtering and recycling catalyst, taking the filtrate, with 30% hydrochloric acid dyeworks to PH1-2, centrifugation after the cooling crystallization, heating precipitation, water washing, to obtain 4-amino -3,6-dichloro-pyridine carboxylic acid 38.8 g, content of 97.5%, yield 91.4%.

References:

Shandong Avilive Chemical Co. Ltd;Zhejiang Avilive Chemical Co., Ltd;Tian, Fengyu;Li, Huiyue;Jin, Keqiang;Gong, Quankai CN105461622, 2016, A Location in patent:Paragraph 0024-0027

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