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Synthetic process of trometamol

A synthesis process, tromethamine technology, applied in the preparation of amino hydroxyl compounds, the preparation of organic compounds, organic chemistry, etc., can solve the problems of relatively high requirements for reaction equipment, low product purity and precision, and high hydrogenation reaction pressure. Achieve the effect of reducing cost and human resource input, reducing equipment requirements, and increasing product yield

Active Publication Date: 2020-09-22
武汉本杰明医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing synthesis process of tromethamine, the pressure of hydrogenation reaction is relatively high, and the requirements for reaction equipment are relatively high, which is easy to cause safety accidents, and the requirements for monitoring personnel are also high.
Moreover, there are many solid and liquid wastes in the process of producing trometamol using the original technology, and there are many three wastes
Simultaneously, the synthesis efficiency of tromethamine has remained unchanged for many years, the synthesis efficiency is not high, and the purity and precision of the product are not high

Method used

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  • Synthetic process of trometamol
  • Synthetic process of trometamol
  • Synthetic process of trometamol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Step 1, synthesis of intermediates: S11: pump nitromethane into a vacuum metering tank for use; S12: pump methanol into a synthesis reaction kettle, add paraformaldehyde under stirring, seal the synthesis reaction kettle, and stir for more than 10 minutes , the material is evenly dispersed; S13: raise the temperature to 35°C, start to add nitromethane and calcium hydroxide dropwise, and control the temperature of the synthesis reactor to 35°C during the dropping process; S14: after the dropwise addition, react at 40°C for 4.5 hours to obtain a mixed liquid; S15: the mixed solution is cooled to room temperature, and sulfuric acid is added to it under controlled room temperature conditions to adjust the pH of the mixed solution to 6; S16: filter, and the filtrate enters the hydrogenation reactor; step 2, the synthesis of the crude product: S21: go to the hydrogenation reaction Continue to add palladium-carbon catalyst to the kettle for hydrogen replacement; S22: Fill in hy...

Embodiment 2

[0036] Step 1, synthesis of intermediates: S11: pump nitromethane into a vacuum metering tank for use; S12: pump methanol into a synthesis reaction kettle, add paraformaldehyde under stirring, seal the synthesis reaction kettle, and stir for more than 10 minutes , the material is evenly dispersed; S13: raise the temperature to 35°C, start to add nitromethane and calcium hydroxide dropwise, and control the temperature of the synthesis reactor to 35°C during the dropping process; S14: after the dropwise addition, react at 40°C for 4.5 hours to obtain a mixed liquid; S15: the mixed solution is cooled to room temperature, and sulfuric acid is added to it under controlled room temperature conditions to adjust the pH of the mixed solution to 6; S16: filter, and the filtrate enters the hydrogenation reactor; step 2, the synthesis of the crude product: S21: go to the hydrogenation reaction Continue to add palladium-carbon catalyst to the kettle for hydrogen replacement; S22: Fill in hy...

Embodiment 3

[0039] Step 1, synthesis of intermediates: S11: pump nitromethane into a vacuum metering tank for use; S12: pump methanol into a synthesis reaction kettle, add paraformaldehyde under stirring, seal the synthesis reaction kettle, and stir for more than 10 minutes , the material is evenly dispersed; S13: raise the temperature to 35°C, start to add nitromethane and calcium hydroxide dropwise, and control the temperature of the synthesis reactor to 35°C during the dropping process; S14: after the dropwise addition, react at 40°C for 4.5 hours to obtain a mixed liquid; S15: the mixed solution is cooled to room temperature, and sulfuric acid is added to it under controlled room temperature conditions to adjust the pH of the mixed solution to 6; S16: filter, and the filtrate enters the hydrogenation reactor; step 2, the synthesis of the crude product: S21: go to the hydrogenation reaction Continue to add palladium-carbon catalyst to the kettle for hydrogen replacement; S22: Fill in hy...

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Abstract

The invention discloses a tromethamine synthesis process. The tromethamine synthesis process comprises the following steps: step 1, synthesizing an intermediate: S11: pumping nitromethane into a vacuum metering tank for later use; S12: pumping methyl alcohol into a synthesis reaction kettle, adding paraformaldehyde while stirring, sealing the synthesis reaction kettle, stirring for more than 10 minutes, evenly dispersing the material; S12: raising the temperature to 35 DEG C, starting to add nitromethane and calcium hydroxide dropwise, controlling the temperature of the synthesis reaction kettle to 30-40 DEG C in the process of adding dropwise; S14: finishing adding dropwise, reacting at the temperature of 40 DEG C for 4.5-5 hours to obtain a mixed solution; S15: cooling the mixed solutionto the room temperature, adding sulfuric acid under the condition that the room temperature is controlled, regulating the pH of the mixed solution to 6-7; S16: filtering, enabling a filtrate to entera hydrogenation kettle; step 2, synthesizing a crude product; and step 3, refining the product. The tromethamine synthesis process has the advantages of safety, environmental protection, high productyield and the like, and is widely applied to the technical field of synthesis of tromethamine.

Description

technical field [0001] The invention relates to the technical field of synthesis of tromethamine. More specifically, the present invention relates to a kind of synthetic technique of tromethamine. Background technique [0002] Tromethamine, a non-sodium amino buffered base. It can react with water in body fluids to reduce it. It is suitable for metabolic acidemia and respiratory acidemia. It is ideal for patients with metabolic acidemia combined with acute respiratory acidemia. Drugs are also important pharmaceutical intermediates. [0003] In the industrial synthesis of tromethamine, the two-step polymerization-hydrogenation method is often used to synthesize tromethamine. However, in the existing trometamol synthesis process, the pressure of the hydrogenation reaction is relatively high, and the requirements for the reaction equipment are relatively high, which is easy to cause safety accidents, and the requirements for monitoring personnel are also high. Moreover, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C215/10
CPCC07C201/12C07C213/02C07C205/15C07C215/10
Inventor 朱桂锋
Owner 武汉本杰明医药股份有限公司
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