Preparation method of o-nitrobenzaldehyde
A technology of o-nitrobenzaldehyde and o-nitroethylbenzene, which is applied in the field of preparation of o-nitrobenzaldehyde, can solve the problems of limiting the safe production of o-nitrobenzaldehyde, difficulties in olefins, and harsh conditions, and achieve raw material Inexpensive, high selectivity, less side effects
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[0015] The embodiment of the present invention provides a kind of preparation method of o-nitrobenzaldehyde comprising the following steps:
[0016] (A) o-nitroethylbenzene carries out oxidation reaction, obtains 1-(2-nitrophenyl) ethanol;
[0017] (B) 1-(2-nitrophenyl) ethanol carries out oxidation reaction, obtains o-nitroacetophenone;
[0018] (C) O-nitroacetophenone is oxidized to obtain o-nitrobenzaldehyde.
[0019] The preparation method of o-nitrobenzaldehyde provided by the invention uses o-nitroethylbenzene as a raw material, and undergoes three steps of oxidation reactions under different conditions to obtain o-nitrobenzaldehyde, and the total yield can reach more than 60%. The preparation method has reasonable route, cheap raw materials, can effectively control production cost, has high yield and high product purity. The preparation process of the invention not only avoids the use of bromine and nitric acid, but also greatly reduces the generation of waste water, ...
Embodiment 1
[0056] The present embodiment provides a kind of preparation method of o-nitrobenzaldehyde, and its synthetic route is as follows,
[0057]
[0058] Concrete preparation method comprises the following steps:
[0059] (A) Add 3.021 g of o-nitroethylbenzene, 0.080 g of sodium hydroxide and 30 ml of diethylene glycol dimethyl ether into a reaction vessel, blow in air, heat to 115° C., and react for 10 hours. After the reaction, the reaction solution was cooled, added deionized water, and then extracted with methyl tert-butyl ether to obtain a water layer and a methyl tert-butyl ether layer. After separation, the aqueous layer was concentrated to remove water and the solvent diethylene diethyl ether Alcohol dimethyl ether can continue to be recycled, and the methyl tert-butyl ether layer is distilled to obtain a crude product (3.520 g, a purity of 81.6%, converted to a pure product of 2.872 g, a yield of 86.0%) for direct use in the next reaction.
[0060] (B) Mix the crude pr...
Embodiment 2
[0063] The present embodiment provides a kind of preparation method of o-nitrobenzaldehyde, and specific preparation method comprises the following steps:
[0064] (A) Add 1.82g of o-nitroethylbenzene, 3.60g of sodium hydroxide, 16mL of ethanol and 4mL of water into a reaction vessel, blow in air, heat to 65°C, and stir for 24 hours. After the reaction, the reaction solution was cooled, and 40 mL of deionized water was added, then extracted with 60 mL of dichloroethane to obtain an aqueous solution layer of ethanol and an ethylene dichloride layer. After separation, the aqueous solution layer of ethanol was distilled to reclaim ethanol, and the ethanol recovered could be Continue to recycle, and the dichloroethane extract is directly used for the next step reaction.
[0065] (B) In the ethylene dichloride extract obtained in step (A), add ferric nitrate nonahydrate 0.484, sodium chloride 0.070 and tetramethylpiperidine nitride (TEMPO) 0.094g, feed oxygen, be heated to 60 ° C,...
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