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Method for synthesizing dihydrosafrole

A technology of dihydrosafrole and a synthesis method, applied in the field of synthesis of dihydrosafrole, can solve problems such as depletion of raw materials, and achieve the effects of less three wastes, easy handling and reduction of side reactions

Inactive Publication Date: 2007-02-07
贵阳海丰精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It also leads to the depletion of raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) ring closure

[0022] The ring closure reaction equipment is a device with stirring, reflux and steam distillation device.

[0023] First put 1.4kg of sodium hydroxide into the ring-closure reactor, then add 3.5kg of solvent dimethyl sulfoxide, then add 1.2kg of dichloromethane, start stirring, and heat up; get catechol 1.6kg and dissolve it in 1.5 kg dimethyl sulfoxide for standby;

[0024] When the temperature rises to 90°C, slowly add the dissolved catechol dimethyl sulfoxide solution into the reactor, and control the temperature at 90°C-110°C. After the addition is completed within about 2 hours, let the reaction continue Finish reaction after about 2 hours, then cool down;

[0025] After the material is cooled, filter out the salt generated by the reaction, put the liquid material into a steam distillation device for distillation, collect the product after 90°C, and obtain about 1.7kg of the intermediate product piperonine with a content of about 95%;

[002...

Embodiment 2

[0036] (1) ring closure

[0037] The ring closure reaction equipment is a device with stirring, reflux and steam distillation device.

[0038] First put 1.3kg of sodium hydroxide into the cyclization reactor, then add 3.15kg of solvent dimethyl sulfoxide, then add 1.1kg of dichloromethane, start stirring, and heat up; take catechol 1.4kg and dissolve it in 1.35 kg dimethyl sulfoxide for standby;

[0039] When the temperature rises to 90°C, slowly add the dissolved catechol dimethyl sulfoxide solution into the reactor, and control the temperature at 90°C-110°C. After the addition is completed within about 2 hours, let the reaction continue Finish reaction after about 2 hours, then cool down;

[0040] After the material is cooled, filter out the salt generated by the reaction, put the liquid material into a steam distillation device for distillation, collect the product after 90°C, and obtain about 1.7kg of the intermediate product piperonine with a content of about 95%;

[0...

Embodiment 3

[0051] (1) ring closure

[0052] The ring closure reaction equipment is a device with stirring, reflux and steam distillation device.

[0053] First put 1.6kg of sodium hydroxide into the ring-closure reactor, then add 3.85kg of solvent dimethyl sulfoxide, then add 1.4kg of dichloromethane, start stirring, and heat up; take catechol 1.6kg and dissolve it in 1.65 kg dimethyl sulfoxide for standby;

[0054] When the temperature rises to 90°C, slowly add the dissolved catechol dimethyl sulfoxide solution into the reactor, and control the temperature at 90°C-110°C. After the addition is completed within about 2.5 hours, let the reaction continue Finish the reaction after about 2.5 hours, then cool down;

[0055] After the material is cooled, filter out the salt generated by the reaction, put the liquid material into a steam distillation device for distillation, collect the product after 90°C, and obtain about 1.7kg of the intermediate product piperonine with a content of about 9...

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Abstract

The invention discloses a synthesizing method of dihydrosafrole, which comprises the following steps: ringing catechol; proceeding Friedel-Crafts acyl reaction and Clemmensen reduction; distilling to produce the product with over 95% content.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for synthesizing dihydrosafrole. Background technique [0002] Dihydrohydrosafrole, chemical name: 3,4-methylenedioxypropylbenzene, English name: Dihydrosafrole, colorless clear liquid, has a smell similar to safrole, refractive index (n20D): 1.5170~1.5200, relative density (D25): 1.065-1.075. Dihydrosafrole is an important fine chemical raw material, which is widely used in the synthesis of chemical products such as flavors and fragrances, pharmaceutical intermediates, food additives and pesticides, especially in the synthesis of pesticide synergist piperonyl butoxide; The sharp increase in demand for dihydrosafrole has led to a constant rise in its price. Due to the development of economy and society in recent years, natural resources—especially natural plant resources have been exploited unprecedentedly. Driven by economic interests, a large number of natural plant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/50
Inventor 杜云兴申东升罗明
Owner 贵阳海丰精细化工有限公司
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