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Synthesis method of methyl phenylacetate

A technology of methyl phenylacetate and synthesis method, applied in the chemical field, can solve the problems of low purity and low yield of methyl phenylacetate, and achieve the effect of good purity and high yield

Pending Publication Date: 2022-01-11
宁夏常晟药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the purity of the methyl phenylacetate of present synthesis is low, and yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] A kind of synthetic method of methyl phenylacetate, is characterized in that, this synthetic method comprises the steps:

[0014] (1) According to the mass ratio of methanol, benzyl chloride, catalyst, and 35% sodium cyanide aqueous solution with a mass fraction of 15:4~6:0.01:4, the material is taken, and methanol, benzyl chloride, and catalyst are put into the reaction In the kettle, raise the temperature to 40-45°C, add dropwise a 35% sodium cyanide aqueous solution, cool down, add dichloromethane for extraction, let stand to separate layers, remove the oil layer, and transfer the water layer to the cyanide breaking kettle for cyanide breaking treatment , to obtain phenylacetonitrile; the catalyst is benzyltriethylammonium chloride;

[0015] (2) According to the mass ratio of phenylacetonitrile and hydrogen chloride methanol to 3-5:16, take materials, put phenylacetonitrile and hydrogen chloride methanol into the reaction kettle, heat up to 55°C, keep warm, heat up t...

Embodiment 1

[0017] A kind of synthetic method of methyl phenylacetate, is characterized in that, this synthetic method comprises the steps:

[0018] (1) Put 1500kg of methanol, 400kg of benzyl chloride, and 1kg of catalyst into the reactor, heat up to 40-45°C, add 400kg of aqueous sodium cyanide solution with a mass fraction of 35%, drop the temperature to room temperature, add dichloromethane for extraction, Stand for stratification, remove the oil layer, transfer the water layer to the cyanide breaking tank for cyanide breaking treatment, extract the obtained organic solvent layer, transfer it to the washing tank, wash with water, and then transfer it to the distillation tank for solvent recovery after dehydration. Carry out high vacuum decompression distillation then, obtain 278kg benzyl cyanide, purity 96.9%; Catalyst is benzyl triethyl ammonium chloride;

[0019] (2) Put 300kg of phenylacetonitrile and 1600kg of hydrogen chloride methanol into the reaction kettle, raise the temperatu...

Embodiment 2

[0022] A kind of synthetic method of methyl phenylacetate, is characterized in that, this synthetic method comprises the steps:

[0023] (1) Put 1500kg of methanol, 500kg of benzyl chloride, and 1kg of catalyst into a reaction kettle, raise the temperature to 40°C, add a 35% sodium cyanide aqueous solution dropwise, cool down to room temperature, add dichloromethane for extraction, and let stand to separate Separate the oil layer, the water layer is transferred to the cyanide breaking tank for cyanide breaking treatment, the organic solvent layer extracted is transferred to the washing tank, washed with water, and then dehydrated, then transferred to the distillation tank for solvent recovery, and then high Distilled under reduced pressure in vacuum to obtain 301kg of phenylacetonitrile with a purity of 98.8%; the catalyst was benzyltriethylammonium chloride;

[0024] (2) Take materials according to the mass ratio of phenylacetonitrile and hydrogen chloride methanol of 3 to 5:...

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Abstract

The invention belongs to the field of chemistry, and particularly relates to a synthetic method of methyl phenylacetate. According to the method, benzyl chloride and the like are used as raw materials, methyl phenylacetate is prepared through substitution reaction and addition reaction, and the synthetic product is high in yield and good in purity.

Description

Technical field [0001] The invention belongs to the field of chemistry, and specifically relates to a synthesis method of methyl phenylacetate. Background technique [0002] Methyl phenylacetate, also known as α-methyl toluate. Found naturally in cocoa, coffee and strawberries. Colorless to light yellow oily liquid with a weak honey and musk-like aroma and a slight sweetness. It can be used as spices in cosmetics, detergents, soaps and room fresheners, and to prepare cigarette flavors. It can also be used to prepare honey, chocolate and other flavors, used in food, and can also be used in medicines and organic synthesis intermediates. However, the currently synthesized methyl phenylacetate has low purity and low yield. Contents of the invention [0003] In view of the above problems, the present invention provides a synthesis method of methyl phenylacetate. [0004] A synthetic method of methyl phenylacetate, characterized in that the synthetic method includes the foll...

Claims

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Application Information

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IPC IPC(8): C07C67/22C07C69/614C07C253/14C07C255/33
CPCC07C67/22C07C253/14C07C255/33C07C69/614
Inventor 陈健龙代良月金璐仪
Owner 宁夏常晟药业有限公司
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