Production process of p-nitrobenzyl alcohol

Abstract

The invention relates to the field of drug intermediates, and particularly discloses a production process of p-nitrobenzyl alcohol, which comprises the following steps: S1, bromination reaction: putting p-nitrotoluene and water into a reaction kettle, stirring, heating to 40-55 DEG C, dropwise adding bromine, dropwise adding an initiator in batches, and carrying out heat preservation reaction after the initiator is dropwise added; s2, whitening and hydrolysis reaction: adding sodium sulfite to whiten, stirring, adding water, heating, refluxing and hydrolyzing for 4-10 hours, cooling to below 70 DEG C, and adding sodium carbonate to adjust the pH value; and S3, separating, adding a solvent into the reaction product obtained in the step S2, standing for layering to obtain an oil solution layer and a water solution layer, and concentrating, cooling, crystallizing and filtering the oil solution layer to obtain a p-nitrobenzyl alcohol crude product. According to the production process, the heat energy consumption is low, the yield is improved after the catalyst is added, the production efficiency is improved, the reaction heating time is further shortened, the heat energy consumption is low, and the safety is good.

Description

technical field [0001] The application relates to the technical field of pharmaceutical intermediates, and more specifically, to a production process of p-nitrobenzyl alcohol. Background technique [0002] p-Nitrobenzyl alcohol, also known as 4-nitrobenzyl alcohol or p-nitrobenzyl alcohol, is an important fine chemical. Nitroacetate p-nitrobenzyl alcohol ester, p-nitrobenzyl alcohol malonate monoester, meropenem side chain, etc. all need to use p-nitrobenzyl alcohol as the starting material. [0003] Patent CN104370746 discloses that p-nitrotoluene is used as raw material, p-nitrobenzyl chloride is obtained by chlorination, and p-nitrobenzyl alcohol is obtained through purification, alkaline hydrolysis, distillation and other steps. [0004] In view of the above-mentioned related technologies, the inventors believe that in the production process, most steps require relatively high temperatures, wherein the chlorine gas introduction temperature is 150-180°C, the steam distil...

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Problems solved by technology

[0004] In view of the related technologies mentioned above, the inventor believes that in the production process, most of the steps require relatively high temperatures, among which, the chlorine gas introduction temperature is 150-180°C, the steam distillation temperature is 100-200°C, and repeated distillation is required in the follow-up In order to produce p-nitrobenzyl alcohol, the heat energy consumption is high and the production cost is high

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