Method for preparing propargyl alcohol by using micro-structural reactor

A microstructure reactor, propargyl alcohol technology, applied in the direction of organic Grignard reaction, chemical instruments and methods, organic chemical methods, etc., can solve the problem of unreported propargyl alcohol, and achieve high selectivity and mild reaction conditions. , the effect of simple operation

Inactive Publication Date: 2014-07-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation of Grignard reagents in microstructured reactors has been reported (Wakami H.; Yoshida J.Org.Process.Res.Dev.2005, 9...

Method used

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  • Method for preparing propargyl alcohol by using micro-structural reactor
  • Method for preparing propargyl alcohol by using micro-structural reactor

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Experimental program
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Embodiment 1

[0026] Such as figure 1 Shown: Ethylmagnesium bromide is injected into micromixer B1 (cross-toed micromixer, HPIMM, IMM, Germany, length×width×height=25×21×37μm) from high-pressure syringe pump A1 and metered into acetylene by F Gas reaction, the gas flow rate ratio of ethylmagnesium bromide to acetylene is 1:300, Grignard exchange reaction occurs in thermostat D1 (0°C), enters microchannel reactor C1 (inner diameter: 1mm) and continues to react for 10s, the product ethynyl Magnesium bromide is pumped into micro-mixer B2 (V2, IMM, Germany) by plunger pump A4 and mixed with tetrahydrofuran mixture (0.1mol / L) of benzaldehyde pumped by high-pressure syringe pump A2 in thermostat D2 (25°C) , the molar ratio of Grignard reagent to benzaldehyde is 1:1, and then enter the microchannel reactor C2 (inner diameter: 1mm) to continue the reaction for 20s, and the obtained product enters the micromixer B3 (T-type tee, inner diameter: 1mm) React with ammonium chloride solution pumped by sy...

Embodiment 2

[0028] Such as figure 1 Shown: Ethylmagnesium bromide is injected into micro-mixer B1 (Caterpillar, IMM, Germany, length×width=300×300μm) from high-pressure syringe pump A1 to react with acetylene gas metered by F, and the ratio of ethylmagnesium bromide to acetylene gas The flow rate ratio is 1:100, the Grignard exchange reaction occurs in the incubator D1 (0°C), and enters the microchannel reactor C1 (inner diameter: 0.5mm) to continue the reaction for 5s, and the product ethynylmagnesium bromide is pumped into the microchannel reactor by the plunger pump A4. Mixer B2 (cross-toed micro-mixer, HPIMM, IMM, Germany, length × width × height = 25 × 21 × 37 μm) and the tetrahydrofuran mixture (1mol / L) of benzaldehyde pumped by high-pressure syringe pump A2 were kept at constant temperature Mix in box D2 (25°C), the molar ratio of Grignard reagent to benzaldehyde is 1:1.2, and then enter the microchannel reactor C2 (inner diameter: 1mm) to continue the reaction for 6s, and the obta...

Embodiment 3

[0030]As shown in the figure: Ethylmagnesium bromide is injected into falling film microstructure reactor B1 (length×width: 300×100μm) from high-pressure injection pump A1 to react with acetylene gas metered by F, and the flow rate of ethylmagnesium bromide is higher than that of acetylene gas Ratio 1:50, Grignard exchange reaction occurs in thermostat D1 (0°C), enters microchannel reactor C1 (inner diameter: 3mm) and continues to react for 2 minutes, and the product ethynylmagnesium bromide is pumped into the micromixer by plunger pump A4 B2 (T-type tee, inner diameter: 1mm) is mixed with the tetrahydrofuran mixture (3mol / L) of benzaldehyde pumped by the high-pressure syringe pump A2 in the incubator D2 (25°C), and the moles of Grignard reagent and benzaldehyde The ratio is 1:0.8, and then enter the microchannel reactor C2 (inner diameter: 1mm) to continue the reaction for 2 minutes, and the obtained product enters the micro-mixer B3 (T-type tee, inner diameter: 6mm) and is pu...

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Abstract

The invention provides a method for preparing propargyl alcohol by using a micro-structural reactor, which comprises the steps of by taking a simple Grignard reagent as a raw material, carrying out gas-liquid Grignard exchange reaction on the simple Grignard reagent and acetylene gas to generate a high-quality acetylene-based magnesium bromide Grignard reagent, carrying out nucleophilic addition reaction on the obtained acetylene-based magnesium bromide Grignard reagent and an electrophilic reagent in a continuous flow condition, and carrying out hydrolysis, separation and refining on the product to obtain a substitution propargyl alcohol product. The method provided by the invention has the advantages that the operation is simple, the raw material and the reagent are simple, cheap and easily available, the process is continuous, rapid and controllable, the condition is mild, the product has good selectivity and industrial production can be realized.

Description

technical field [0001] The invention relates to a method for preparing propargyl alcohol, in particular to a method for preparing propargyl alcohol using a microstructure reactor. Background technique [0002] Substituted propargyl alcohols with the following structure are important synthetic intermediates, which are mainly used in the fields of medicine and synthetic materials, and can also be used as glazing agents for nickel plating or copper. Under the conditions of high temperature, high pressure and concentrated acid, propargyl alcohol has good ability to prevent metal corrosion. [0003] [0004] The synthesis method of Chinese patent CN102701911A mainly includes passing dry acetylene gas into Grignard reagent or lithium reagent at low temperature (-78°C) for Grignard exchange, or passing sodium amide or lithium amide under liquid ammonia environment In, or into the tetrahydrofuran solution of potassium tert-butoxide, and then slowly drop the ketone or aldehyde in...

Claims

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Application Information

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IPC IPC(8): C07C33/30C07C33/48C07C33/38C07C33/14C07C33/042C07C29/42C07C43/23C07C41/30C07B49/00
CPCC07C29/42C07C41/30C07C2601/14C07C2603/18C07C33/30C07C43/23C07C33/483C07C33/38C07C33/14C07C33/042
Inventor 张利雄邓秋林沈如伟
Owner NANJING UNIV OF TECH
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