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A kind of synthetic technique of salicylaldehyde

A synthesis process and salicylaldehyde technology, applied in the field of salicylaldehyde synthesis technology, can solve the problems of low yield rate, large environmental pollution and high production cost in the production process, and achieve good economic and social benefits, high purity and high cost low effect

Active Publication Date: 2015-09-09
XIANTAO XIANSHENG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of this invention is to provide a kind of synthesis process of salicylaldehyde, to solve the technical problems such as low yield rate, high production cost, use of toxic solvents, and large environmental pollution in the existing salicylaldehyde production process

Method used

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  • A kind of synthetic technique of salicylaldehyde

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Embodiment 1

[0016] Embodiment 1: the synthetic technique of this salicylaldehyde comprises the following steps:

[0017] A. Put the 4A molecular sieve in the muffle furnace to activate and remove water for 5 hours at 400°C, and then place it in a desiccator to cool to room temperature; take 0.005 parts (100 grams each, the same below) of 4A molecular sieve and mix with 0.5 parts of methanol , put 0.1 part of metal magnesium and 0.01 part of iodine into the reaction kettle, control the temperature at 40 ° C, stir until the magnesium completely disappears, and obtain a mixed solution containing magnesium methanol and methanol;

[0018] B. Add 0.2 parts of phenol, 0.01 parts of polyvinyl alcohol, and 0.001 parts of N-acyl ED3A to the reaction kettle, continue to stir and heat to 64 ° C, wait for most of the methanol to distill, add 0.9 parts of toluene to the reaction kettle, continue Carry out heating distillation and constant stirring to distill out the azeotrope of toluene and methanol. W...

Embodiment 2

[0022] Embodiment 2: the synthetic technique of this salicylaldehyde comprises the following steps:

[0023] A. Put the 4A molecular sieve in the muffle furnace to activate and remove water for 5 hours at 400°C, and then place it in a desiccator to cool to room temperature; take 0.0055 parts of 4A molecular sieve and mix with 0.55 parts of methanol, add 0.1 parts of magnesium metal and 0.01 parts of iodine Pour parts into the reaction kettle, control the temperature at 40°C, and stir until the magnesium completely disappears to obtain a mixed solution containing magnesium methanol and methanol;

[0024] B. Add 0.25 parts of phenol, 0.02 parts of polyvinyl alcohol, and 0.01 parts of N-acyl ED3A to the reaction kettle, continue to stir and heat to 65 ° C, wait for most of the methanol to distill, add 0.94 parts of toluene to the reaction kettle, continue Carry out heating distillation and constant stirring to distill out the azeotrope of toluene and methanol. When the temperatur...

Embodiment 3

[0028] Embodiment 3: the synthetic technique of this salicylaldehyde, comprises the following steps:

[0029] A. Put the 4A molecular sieve in a muffle furnace to activate and remove water for 5 hours at 400°C, and then place it in a desiccator to cool to room temperature; take 0.006 parts of 4A molecular sieve and mix with 0.6 parts of methanol, and mix 0.1 parts of magnesium metal and 0.01 parts of iodine Pour parts into the reaction kettle, control the temperature at 40°C, and stir until the magnesium completely disappears to obtain a mixed solution containing magnesium methanol and methanol;

[0030] B. Add 0.3 parts of phenol, 0.03 parts of polyvinyl alcohol, and 0.02 parts of N-acyl ED3A to the reaction kettle, continue to stir and heat to 66 ° C, wait for most of the methanol to distill, add 0.98 parts of toluene to the reaction kettle, continue Carry out heating distillation and constant stirring to distill out the azeotrope of toluene and methanol. When the temperatur...

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Abstract

The invention discloses a synthetic technology of salicylaldehyde. Toxic solvents such as HMPA are replaced by cheap and easily available reaction raw materials such as phenol and paraformaldehyde; and no toxic substances are generated in reaction processes. According to the synthetic technology, phenol is added into methanol solution of magnesium methoxide, and phenol magnesium is obtained by methanol distillation; because of metal characteristic of magnesium, in reaction processes of phenol magnesium and methanol, coordination reaction of magnesium ions is induced before coordination reaction of methanol, methanol treated by coordination reaction is closes to the ortho-position of phenol, a magnesium salt of salicylaldehyde is generated selectively by electrophilic attack of methanol on the ortho-position of phenol, and salicylaldehyde is obtained by treating the magnesium salt with diluted hydrochloric acid. Cost of the synthetic technology is low, contamination is less, yield is high (>85%), purity is high (>99%), and the synthetic technology possesses excellent economic benefits and social benefits.

Description

technical field [0001] The invention relates to an organic synthesis intermediate, in particular to a synthesis process of salicylaldehyde. Background technique [0002] Salicylaldehyde (Salicylaldehyde) scientific name o-hydroxybenzaldehyde, is a colorless or light yellow liquid, widely used in medicine, pesticide, fragrance, electroplating, petrochemical industry. In recent years, the demand for chlorine-free salicylaldehyde in the pharmaceutical and perfume industries has been increasing, making the research and development of new processes for salicylaldehyde one of the active fields. [0003] The most direct and synthetic route of salicylaldehyde is to introduce a formyl group at the ortho position of phenol, while traditional formylation methods, such as Reimer~Tiemman, ortho-cresol method are the most widely used. However, the traditional production method of salicylaldehyde has a very low yield (less than 60%), which leads to high production costs for enterprises. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/565C07C45/71
CPCC07C45/64C07C45/71C07C47/565
Inventor 邵新华
Owner XIANTAO XIANSHENG FINE CHEM
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