A method for catalytic hydrogenation to synthesize 1-amino-4-methylpiperazine
A methylpiperazine, catalytic hydrogenation technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as inapplicability
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Embodiment 1
[0033]Example 1.PD / FE3O4-FEO load catalyst preparation steps are as follows:
[0034]20 g of hexahydrachloride and 20 g of tetrahydride of ferrous chloride were added to a hydrated reaction kettle, and 16 g of polyvinylpyrrolidone was added to 200 ml of ethylene glycol mixed solution, and 15 g of urea and nitrogen were added three times. Heat was heated. 160 ° C for 10 hours, cool, filtered, 500ml deionized water wash 5 times3O4-Feo. 110 mL of a palladium chloride solution of 0.00115 mol / L was taken with 1.4 g of polyvinylpyrrolidone, and 100 ml of 0.1980 mol / L of sodium borohydride solution was added dropwise, and stirring was continued for 4 hours. Put the above Fe3O4-FEO was added to the solution at several hours, was washed with 200 ml of deionized water, and finally was washed with 200 ml of ethanol, and the magnetic Pd / Fe was obtained by vacuum drying at 80 ° C.3O4-Feo. Taking the magnet test catalyst as a paramagnetic property.
Embodiment 2
[0035]Example 2.1-Preparation steps of methyl-4-nitrosipipiperazine are as follows:
[0036]
[0037]200 ml of water was added to 1 L of three bottles, and 250 ml of concentrated hydrochloric acid was added under stirring, and then the ice bath was controlled to reduce N-1-methylpiperazine 100 g below 40 ° C or lower. After the addition was completed, stirring was stirred at a temperature of 20-30 ° C, 72.5 g of sodium nitrite was added to the system. After the addition, the reaction was continued for 1.5 hours, TLC / GC detection reaction was complete, and 55 ml 30% sodium hydroxide solution was adj to transfer pH = 7 left and right, 1-methyl-4-nitrozine hydration, extracted 2 times in 200 ml of dichloromethane, combined with dichloromethane, evaporation of dichloromethane under reduced pressure 126g pale yellow oily liquid 1 - Methyl-4-nitropiperazine, yield 97%, GC analysis of 98.5%.
Embodiment 3
[0038]Example 3.1 - Preparation steps of methyl-4-nitroidine dichloromethane solution are as follows:
[0039]
[0040]200 ml of water was added to 1 L of three bottles, and 250 ml of concentrated hydrochloric acid was added under stirring, and then the ice bath was controlled to reduce N-1-methylpiperazine 100 g below 40 ° C or lower. After the addition was completed, stirring was stirred at a temperature of 20-30 ° C, 72.5 g of sodium nitrite was added to the system. After the addition, the reaction was continued for 1.5 hours, TLC / GC detection reaction was complete, and 55 ml 30% sodium hydroxide solution was adj to transfer pH = 7 left and right gave 1-methyl-4-nitrozine hydration, extracted 2 times in 200 ml of dichloromethane, combined with dichloromethane layer, 400 ml of chlorine of 1-methyl-4-nitrozine The methane solution is directly subjected to a process of catalytic hydrogenation, and the GC analysis is 98.5%.
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