Method for synthesizing o-aminoanisole by hydrogenation method

Abstract

The invention discloses a method for synthesizing o-aminoanisole by a hydrogenation method. The synthesis method specifically comprises the following steps: adding metallic sodium to excess methanol to prepare a methanol solution of sodium methoxide, and then spraying o-nitrochlorobenzene and the methanol solution of sodium methoxide into an etherification kettle; firstly, performing centrifugal separation, then transferring to a distillation kettle for distillation, and then crystallizing and filtering; firstly, introducing the hydrogen gas to exhaust the gas, atomizing o-nitroanisole, usinga catalyst for catalyzing the reaction, introducing nitrogen gas to the kettle to exhaust the gas after the reaction is completed, then cooling and crystallizing, centrifuging at low temperature for separation and filtering, and repeatedly operating for 2 to 3 times to obtain o-aminoanisole. The method for synthesizing o-aminoanisole by the hydrogenation method uses nitrogen-doped porous carbon asa carrier for the catalyst, and the catalyst is made into a lattice. Contact area of the reactant is large, and the reaction proceeds rapidly. A methoxy reagent is directly prepared from the metallicsodium and methanol, and the methoxy reagent is dissolved with methanol to prepare a solution for spraying, so as to accelerate the reaction and promote the reaction to proceed forward.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing anthranil by hydrogenation. Background technique [0002] Anthranilic acid is an important chemical intermediate, which is widely used in the production of dyes, pesticides, medicines and other fields. Since aniline and sulfuric acid are salted and translocated to generate p-aminobenzenesulfonic acid, the current domestic preparation method is o-chloronitrobenzene and Sodium disulfide is co-heated in alcohol to convert it into 2,2-dinitrodiphenyl disulfide, then oxidize it with chlorine gas into o-nitrobenzenesulfonyl chloride, hydrolyze it into o-nitrobenzenesulfonic acid with sodium carbonate, and then use iron powder or hydrogenation reduction of nitro into amino groups to obtain o-aminobenzenesulfonic acid, CN101362710, CN1066446, Chemical Production and Technology (2009), 16(4), 23-24. Sulfonated to generate o-nitrobenzenesulfonic acid, a...

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Problems solved by technology

[0003] The disadvantages of the above process are long route, large amount of three wastes, and low yield. Although the nitro hydrogenation reduction process replaces the iron powder reduction process, it can only reduce part of the th

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