Tubular reactor of 3-hydroxytetrahydrofuran

Abstract

The invention belongs to the technical field of production of pharmaceutical intermediates, and particularly relates to a tubular reactor of 3-hydroxytetrahydrofuran. The tubular reactor comprises a material storing device and a controllable feeding device, wherein the material storing device comprises a malic acid solution batching tank and a sodium borohydride suspension batching tank; the controllable feeding device comprises a PLC controller, output pumps and flow meters which are connected through signals; the PLC controller is provided with a signal input end and a signal output end; andthe controllable feeding device is arranged on output pipes of the malic acid solution batching tank and the sodium borohydride suspension batching tank. By controlling the proportion and amount of raw materials, excessive use of sodium borohydride is avoided, therefore, the consumption of sodium borohydride is reduced and a safety risk caused by hydrogen is avoided; the tubular reactor is placedin a water bath, materials are introduced into a reaction spiral tube after being mixed, and the environment temperature rises rapidly to the reaction temperature, so that the rapid reaction of the materials is achieved, changes of the overall environment temperature are reduced, and the safe and stable reaction can be guaranteed.

Description

technical field [0001] The invention belongs to the technical field of production of pharmaceutical intermediates, and in particular relates to a tubular reactor for 3-hydroxytetrahydrofuran. Background technique [0002] 3-Hydroxytetrahydrofuran is used more and more in pharmaceutical products, among which the main downstream products of S-3-Hydroxytetrahydrofuran are fosamprenavir (for the treatment of AIDS), empagliflozin (for the treatment of diabetes), a Fatinib (anticancer drug), R-3-hydroxytetrahydrofuran (used in the treatment of pfize Alzheimer's disease), it can be seen that 3-hydroxytetrahydrofuran is a versatile intermediate, with the listing, the demand for 3-hydroxytetrahydrofuran will also expand. [0003] However, there are insurmountable limiting factors in the existing production process. At present, starting from dimethyl malate and obtaining 1,2,4-butanetriol through NaBH4 reduction, all adopt kettle-type intermittent reaction. In order to ensure the com...

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Problems solved by technology

[0003] However, there are insurmountable limiting factors in the existing production process. At present, starting from dimethyl malate and obtaining 1,2,4-butanetriol through NaBH4 reduction, all adopt kettle-type intermittent reaction. In order to ensure the complete reaction, the process A large excess of sodium borohydride is used in the process. Methanol is used as a reaction solvent to decompose sodium borohydride very quickly at room temperature. It not only consumes sodium borohydride, but also decomposes to generate a large amount of hydrogen, causing safety risks; Sodium hydride is added to the reaction liquid and mixed with dimethyl malate, and then the temperature is raised to the reaction temperature. Since the reduction reaction is a violent exothermic reaction, the reaction temperature rises sharply. After the temperature rises, the reaction speed is further accelerated, thereby further releasing a large amount of heat, forming a vicious circle, and the reaction is facing out of control; however, the optimal reaction temperature for this reaction is 60-65°C, if the temperature is too high, it will exceed the boiling point of methanol, and it will become a punch, or even catch fire and explode; if the reaction temperature is too low, the reaction will not be complete. It is becoming waste; so in order to control the risk, the reaction can only be carried out in small batches and multiple batches, which greatly limits the production capacity; however, each batch of reaction makes the operator thrilling

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