Preparation method for methylamine reaction

Abstract

The invention relates to the technical field of methylation reaction, and discloses a preparation method of methylation reaction, the preparation method comprises the following steps: S1, adding a parachlorobenzoyl L-glutamic acid refined product, a methylamine aqueous solution and cuprous chloride into a microreactor; s2, cooling to room temperature, and discharging to obtain a p-methylaminobenzoyl L-glutamic acid solution; s3, transferring the p-methylaminobenzoyl L-glutamic acid solution into a reaction kettle, firstly adding water and a NaOH solution, and then adding sodium sulfide; s4, carrying out reduced pressure distillation on the filtrate until about 2V of water is left; s5, adding water and zinc chloride into another reaction kettle, and adding concentrated hydrochloric acid; s6, dropwise adding the concentrated solution and concentrated hydrochloric acid, and maintaining the pH value to be 2.0; s7, stirring at room temperature for 0.5 h, adding activated carbon, and continuously stirring; s8, filtering; and S9, continuously stirring for 1 hour, filtering, and drying at 70-80 DEG C, thereby obtaining the product. According to the preparation method of the methylamination reaction, the microreactor is adopted to replace a conventional reaction kettle for reaction, so that the conditions of short process time, high efficiency, high yield, good quality and few three wastes are realized.

Description

technical field [0001] The invention relates to the technical field of methylation reaction, in particular to a preparation method of methylation reaction. Background technique [0002] Methylamine, with a chemical formula of CH5N and a molecular weight of 31.06, is an organic compound and an important organic chemical raw material. It is low-toxic and can form explosive mixtures when mixed with air. Its aqueous solution is a strong base, which is a component of ammonia. A derivative formed after a hydrogen is replaced by a methyl group. Methylamine is the simplest primary amine. Commercially available products are generally its methanol, ethanol, tetrahydrofuran or aqueous solution, or stored as anhydrous gas in a metal tank under pressure. Industrial Products are often transported by trailer after pressurized anhydrous gas, which has a strong fishy smell. [0003] Methotrexate is an anti-folate antineoplastic drug, which mainly inhibits the synthesis of tumor cells by inh...

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Problems solved by technology

[0006] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing a methylation reaction. By adopting a microreactor to replace a traditional conventional reactor for the reaction, it is solved that when the conventional reactor is used for the reaction, the reaction time will be long, There are many impurities and low yield, which eventually leads to the problem of low efficiency. By using microreactors, the advantages of short process time, high efficiency, high yield, good quality and less waste are solved, which solves the problem of traditional conventional reactors. In the process of carrying out the reaction, there will be a long time, many impurities, and low yield, which will lead to the problem of low yield

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