A kind of preparation method of phosphoramide cattle feed additive
A technology for cattle feed and additives, applied in animal feed, chemical instruments and methods, additional food elements, etc., can solve problems such as increasing production costs, reducing nitrogen utilization, and wasting resources in agriculture and animal husbandry.
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Embodiment 1
[0024]
[0025] In the high-pressure reactor, under the protection of argon, start cooling, the inner temperature is 5-10 °C, add 15 g of 3-chlorophenylacetonitrile into the mixed solution of 50 mL of dichloromethane and 100 mL of dimethyl sulfoxide, and keep the temperature constant. Then add 0.23g of palladium acetate, 0.17g of silver acetate and 0.27g of sodium trifluoroacetate, add 12g of sodium hydride (the content is 60%); keep the inner temperature at 10-20°C and stir for 30min, and feed ammonia into the reaction kettle to make The pressure in the kettle reached 0.1 MPa; keep the pressure constant, slowly raise the temperature to 45°C, add 100 mL of ice water to quench the reaction solution after 2 hours of reaction, separate the lower organic phase after standing, and extract the aqueous phase with 100 mL of dichloromethane for several times. The organic phases were combined, dried over anhydrous magnesium sulfate and concentrated to obtain 11 g of 2-(3-chlorophenyl)...
Embodiment 2
[0027]
[0028] In the high-pressure reactor, under the protection of argon, start cooling, and the inner temperature is 5-10 ° C. Add 15 g of 3-chlorophenylacetonitrile into the mixed solution of 20 mL of diiodomethane and 100 mL of dimethyl sulfoxide, and keep the temperature constant. Then add 0.23g of palladium acetate, 0.17g of silver acetate and 0.27g of sodium trifluoroacetate, add 12g of sodium hydride (the content is 60%); The pressure in the kettle reached 0.1 MPa; keep the pressure constant, slowly raise the temperature to 45°C, add 100 mL of ice water to quench the reaction solution after 2 hours of reaction, separate the lower organic phase after standing, and extract the aqueous phase with 100 mL of dichloromethane for several times. The organic phases were combined, dried over anhydrous magnesium sulfate and concentrated to obtain 17 g of 2-(3-chlorophenyl)-2-cyanoethylamine; 1 H NMR (400M, CDCl 3):7.61(s,1H),7.33(d,J=8.0Hz,1H),7.26(s,1H),7.12(d,J=4.0Hz,1H),...
Embodiment 3
[0030]
[0031] In the high-pressure reactor, under the protection of argon, start cooling, and the inner temperature is 5-10 ° C. Add 15 g of 3-chlorophenylacetonitrile into the mixed solution of 20 mL of diiodomethane and 100 mL of dimethyl sulfoxide, and keep the temperature constant. Then add 0.23 g of palladium acetate, 0.17 g of silver acetate and 0.27 g of sodium trifluoroacetate, add 8 g of sodium hydride (the content is 60%); The pressure in the kettle reached 0.1 MPa; keep the pressure constant, slowly raise the temperature to 45°C, add 100 mL of ice water to quench the reaction solution after 2 hours of reaction, separate the lower organic phase after standing, and extract the aqueous phase with 100 mL of dichloromethane for several times. The organic phases were combined, dried over anhydrous magnesium sulfate and concentrated to obtain 14 g of 2-(3-chlorophenyl)-2-cyanoethylamine; 1 H NMR (400M, CDCl 3 ):7.61(s,1H),7.33(d,J=8.0Hz,1H),7.26(s,1H),7.12(d,J=4.0Hz,...
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