A kind of method for preparing ortho esters by phase transfer catalysis in microstructure reactor

A technology of microstructure reactor and phase transfer catalysis, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high safety hazards, long cycle time, high cost, etc., and achieve high safety and reaction The effect of short time and convenient operation

Inactive Publication Date: 2015-09-02
NANJING TECH UNIV
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  • Abstract
  • Description
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Problems solved by technology

[0006] The purpose of the present invention is to provide a phase transfer catalysis method in a microstructure reactor for the preparation of raw esters in view of the disadvantages of low yield, long cycle, high cost, large pollution, and high safety hazards in the preparation process of raw esters. method to achieve low energy consumption and continuous production process

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  • A kind of method for preparing ortho esters by phase transfer catalysis in microstructure reactor
  • A kind of method for preparing ortho esters by phase transfer catalysis in microstructure reactor

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Embodiment 1

[0017] The schematic diagram of the preparation of the original esters in this embodiment is as follows figure 1 As shown, mix chloroform, ethanol and cetyltrimethylammonium bromide evenly, cetyltrimethylammonium bromide is 5% of the ethanol mass, and configure 30% mass concentration of sodium hydroxide Solution, chloroform, ethanol and sodium hydroxide are fed according to the molar ratio of 0.75:1:4, and the raw materials are pumped into the microstructure reactor whose temperature is controlled at 60°C by the high performance liquid chromatography pump, and the micromixer is used for changing Thermal mixer (SIMHEX, IMM, Germany), the channel size is 25×25×20 (μm) (length*width*height), the residence time extension tube uses 25m inner diameter of 0.5mm, FEP tube, the reaction time is controlled at After 15 minutes, the obtained reaction product entered the high-pressure collection kettle, and the pressure of the reaction system was controlled at 2 MPa. The collected product...

Embodiment 2

[0019] Mix 1,1,1-trichloroethane, ethanol and cetyltrimethylammonium bromide evenly, cetyltrimethylammonium bromide is 2% of the mass of ethanol, and configure 40% mass concentration The sodium hydroxide solution, 1,1,1-trichloroethane, ethanol and sodium hydroxide are fed according to the molar ratio of 1.5:1:1, and the raw materials are pumped into the room with a temperature controlled at 80°C by a high performance liquid chromatography pump. In the micro-structure reactor, the micro-mixer is a cross-toed mixer (HPIMM, IMM, Germany), its channel size is 25×21×37 (μm) (length*width*height), and the residence time extension tube uses 10m inner diameter 1.0mm, FEP tube, the obtained reaction product enters the high-pressure collection kettle, and the pressure of the reaction system is controlled at 0.4MPa. The collected product is first filtered to remove sodium chloride, the filtrate is extracted with chloroform, and the organic phase is distilled to obtain the product trieth...

Embodiment 3

[0021] Mix chloroform, methanol and cetyltrimethylammonium bromide evenly, cetyltrimethylammonium bromide is 8% of the quality of methanol, and configure a 45% mass concentration of sodium hydroxide solution, three Chloromethane, methanol and sodium hydroxide are fed in a molar ratio of 2.5:1:5, and the raw materials are pumped into the microstructure reactor with a temperature controlled at 40°C by a high performance liquid chromatography pump, and the micromixer is a T-type mixer (mikroglas, Germany), the channel size is 200×25 (μm) (width*height), the residence time extension tube uses 5m stainless steel 316L tube with inner diameter of 0.5mm and 2m inner diameter of 6mm, the reaction time is controlled at 60min, the obtained reaction The product enters the high-pressure collection kettle, and the pressure of the reaction system is controlled at 4MPa. The collected product is first filtered to remove sodium chloride, the filtrate is extracted with chloroform, and the organi...

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Abstract

The invention relates to a method for preparing ortho-esters in a microstructural reactor via a phase-transfer catalysis process. The method comprises the following steps of: taking multi-halohydrocarbons, lower alcohols and sodium hydroxide as raw materials; taking cetyl trimethyl ammonium bromide as a phase transfer catalyst; and continuously and rapidly preparing ortho-ester products in the microstructural reactor, wherein the products comprise trimethyl orthoformate, triethyl orthoformate, trimethyl orthoacetate and triethyl orthoacetate. According to the method disclosed by the invention, the excellent mass transfer / heat transfer performance of the microstructural reactor is applied to the process of preparing ortho-esters, thus overcoming the key problems of the corrosion of sodium hydroxide on equipment, long reaction cycle, low yield, high cost, high pollution, bad mass transfer effect and the like in the traditional process, and realizing safe and continuous production; and the method has the advantages of being short in reaction time, simple in process, high in product quality, easy to enlarge, and the like.

Description

Technical field: [0001] The present invention relates to a preparation method of a class of organic compounds, especially a method for preparing ortho esters by phase transfer catalysis in a microstructure reactor, in which polyhalogenated hydrocarbons, low-carbon alcohols and sodium hydroxide are used as raw materials , A method for preparing orthoester products by phase transfer catalysis. Background technique: [0002] Orthoesters are an important class of pharmaceutical synthesis intermediates and important raw materials for the synthesis of other organic compounds. They are mainly used in the fields of medicine, pesticides and dyes. The production process of raw ester products mainly includes two-step method, one-step method, hydrocyanic acid method (or acetonitrile method), transesterification method and phase transfer catalysis method. The above-mentioned methods have a series of problems such as low yield, long cycle time, high cost, heavy pollution, and high potent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/32C07C41/60
Inventor 张利雄何为沈如伟王重庆
Owner NANJING TECH UNIV
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