Anisonitrile stage ammonia oxidation approach has actually only been reported in the previous Soviet Union and is still in its beginning in China. This approach has the advantages of uncomplicated raw materials, high selectivity, high return of the target item mononitrile, the reaction just requires to be executed in one reactor, short procedure route, a lot less contamination and light poisoning. The results of this reaction, p-toluene formaldehyde and p-toluic acid, are likewise beneficial natural chemical sources. The growth of this procedure has massive monetary worth.
The creation exposes a synthesis method of Anisonitrile, that includes the sticking to actions: (1) Area 20 mL of paraxylene in a response kettle, warmth the reaction pot to 130-135 ° C, and include solvent DMF, energizer and cocatalyst in turn, manage the oxygen feed quantity to 900mL/min, the hydrogen gas feed quantity to 100mL/min, and react for 4-5h: (2) Cool the above feedback option to area temperature, and the transparent anemic crystals gotten are 4-methoxycyanide. Benzene, make use of DMF to clean the acquired crystals 2-3 times, and eliminate the DMF solvent by suction filtering to get 4-methoxycyanobenzene with a purity higher than 90%: today invention utilizes p-methoxytoluene in the fluid stage under common pressure The one-step method of ammonia oxidation to manufacture 4-methoxycyanobenzene has high yield, high item purity and low demands for tools. It gives a remedy for the industrial production of careful oxidation of p-methoxytoluene to manufacture 4-methoxycyanobenzene. A new, much more economical and green strategy.
Speculative operation:
( 1) Take 20 mL of paraxylene and area it in the action kettle, warmth the response pot to 130 ° C, add the solvent N,N-dimethylformamide DMF, motorist and cocatalyst subsequently, the N,N-dimethylformamide The addition amount of methylformamide DMF is 20mL, the enhancement quantity of energizer and cocatalyst are 2.0 g and 10g particularly, manage the oxygen input amount to 900mL/min, the hydrogen input amount to 100mL/min, and respond for 4 hours;
( 2) Cool the above response choice to area temperature, and the clear anemic crystals gotten are 4-methoxycyanobenzene. After washing the acquired crystals two times with DMF, remove the DMF solvent by suction filtration to acquire a purity more than 90 %Anisonitrile.
Anisonitrile stage ammonia oxidation approach has actually only been reported in the previous Soviet Union and is still in its beginning in China. This approach has the advantages of uncomplicated raw materials, high selectivity, high return of the target item mononitrile, the reaction just requires to be executed in one reactor, short procedure route, a lot less contamination and light poisoning. The results of this reaction, p-toluene formaldehyde and p-toluic acid, are likewise beneficial natural chemical sources. The growth of this procedure has massive monetary worth.
The creation exposes a synthesis method of Anisonitrile, that includes the sticking to actions: (1) Area 20 mL of paraxylene in a response kettle, warmth the reaction pot to 130-135 ° C, and include solvent DMF, energizer and cocatalyst in turn, manage the oxygen feed quantity to 900mL/min, the hydrogen gas feed quantity to 100mL/min, and react for 4-5h: (2) Cool the above feedback option to area temperature, and the transparent anemic crystals gotten are 4-methoxycyanide. Benzene, make use of DMF to clean the acquired crystals 2-3 times, and eliminate the DMF solvent by suction filtering to get 4-methoxycyanobenzene with a purity higher than 90%: today invention utilizes p-methoxytoluene in the fluid stage under common pressure The one-step method of ammonia oxidation to manufacture 4-methoxycyanobenzene has high yield, high item purity and low demands for tools. It gives a remedy for the industrial production of careful oxidation of p-methoxytoluene to manufacture 4-methoxycyanobenzene. A new, much more economical and green strategy.
Speculative operation:
( 1) Take 20 mL of paraxylene and area it in the action kettle, warmth the response pot to 130 ° C, add the solvent N,N-dimethylformamide DMF, motorist and cocatalyst subsequently, the N,N-dimethylformamide The addition amount of methylformamide DMF is 20mL, the enhancement quantity of energizer and cocatalyst are 2.0 g and 10g particularly, manage the oxygen input amount to 900mL/min, the hydrogen input amount to 100mL/min, and respond for 4 hours;
( 2) Cool the above response choice to area temperature, and the clear anemic crystals gotten are 4-methoxycyanobenzene. After washing the acquired crystals two times with DMF, remove the DMF solvent by suction filtration to acquire a purity more than 90 %Anisonitrile.
