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Preparation method of benzodioxole

A pepper ring and recycling technology, applied in the direction of organic chemistry, can solve the problems of high price, expensive catalyst, high cost, etc., and achieve the effects of reducing the time required for reaction, realizing green recycling, and reducing the amount of waste water produced

Active Publication Date: 2019-12-13
SUZHOU HOMESUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(2) Using catechol and dichloromethane as raw materials, the phase transfer catalyst is used to catalyze the synthesis of piperonyl ring, but the recovery is difficult, the cost is high, and it will cause serious environmental pollution
(3) Use catechol and dichloromethane as raw materials to synthesize piperonyl ring with a special organic base, but the price is too expensive to be industrialized
(4) Using catechol and dichloromethane as raw materials to synthesize piperonyl rings with non-polar solvents DMF and DMSO as media, there are cases where the solvent reaction temperature is high (about 130°C) and easy to decompose
(5) Using catechol as raw material, using gas phase dichloromethane reaction, there is a serious loss of dichloromethane
(6) Other literatures introduce the use of solvent-free reaction or molecular sieve catalysis, which are difficult to industrialize due to the high cost of special catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 110ml of DMSO, 30ml of dichloromethane, and 56g of sodium hydroxide into a 500ml three-necked flask, heat up to 50°C with microwave heating, and start to add dropwise the solution of 27.5g of catechol dissolved in 110ml of DMSO to control the temperature of the system. When the temperature exceeds 100°C, add dropwise for 5 hours, then add 20ml of dichloromethane dropwise, keep warm at 90°C for half an hour, cool to room temperature, filter to remove sodium chloride, add 400ml of water, and use an oil-water separator to separate the dichloromethane Chloromethane and piperonylcycline are separated until no obvious oil phase is distilled out, and water is recovered by distillation. The distilled water phase is extracted with an appropriate amount of dichloromethane, and the extracted water phase can be recycled. Distill to the top temperature of 100°C, start switching distillation to recover DMSO, the recovered DMSO can be recycled, and the residue is about 10g. The oi...

Embodiment 2

[0021] Put 110ml of DMSO, 30ml of dichloromethane, and 56g of sodium hydroxide into a 500ml three-necked flask, heat up to 50°C with microwave heating, and start to add dropwise the solution of 27.5g of catechol dissolved in 110ml of DMSO to control the temperature of the system. When the temperature exceeds 90°C, add dropwise for 0.5 hours, then add 20ml of dichloromethane dropwise, keep warm at 90°C for half an hour, cool to room temperature, filter to remove sodium chloride, add 400ml of water, and use an oil-water separator to separate the dichloromethane Chloromethane and piperonylcycline are separated until no obvious oil phase is distilled out, and water is recovered by distillation. The distilled water phase is extracted with an appropriate amount of dichloromethane, and the extracted water phase can be recycled. Distill to the top temperature of 100°C, start switching distillation to recover DMSO, the recovered DMSO can be recycled, and the residue is about 10g. The o...

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PUM

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Abstract

The invention discloses a preparation method of benzodioxole. The preparation method comprises the following steps: with DMSO, dichloromethane and sodium hydroxide as base materials, controlling a temperature to be not higher than 100 DEG C in a microwave heating manner, dropwise adding a DMSO solution of catechol, and separating out the product benzodioxole and dichloromethane after a reaction isfinished. The preparation method is low in price, mild in reaction conditions, low in the generation amount of wastewater and good in process safety, can realize green recycling of an organic solvent, and reduces production cost.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of piperonyl cyclocyclene. Background technique [0002] Peppercycline, chemical name 1,2-methylenedioxybenzene, is widely used in the preparation of low-toxicity insecticides, berberine, jasmonal and sesamol, and antioxidants. Its biochemical activity has attracted widespread attention, and the research and development of its preparation technology has become one of the key points in the research of synthetic drugs and synthetic spices. Due to the needs of social development, the preparation technology using plant essential oils as starting materials is increasingly limited by the protection of ecological resources. Research and development of total chemical synthesis process routes using petrochemical products as starting materials has become an urgent requirement for social development. [0003] The synthesis methods introduced in the current literature ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/50
CPCC07D317/50
Inventor 翟金星陆红彬樊超
Owner SUZHOU HOMESUN PHARMA
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