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Method for preparing o-methoxybenzaldehyde by use of micro-reaction device

A technology of o-methoxybenzaldehyde and micro-reaction devices, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of complex processes and low yields, and achieve simple processes and relatively low yields. The effect of large surface area and high operating flexibility

Active Publication Date: 2015-03-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process is complicated and the yield is low, and it has been eliminated at present; ②Chemical synthesis method: According to different sources of raw materials, there are various process routes, such as o-cresol method, anisole method, o-methoxytoluene oxidation method, p-methoxytoluene oxidation method, Hydroxybenzaldehyde methylation method, etc., each method has its advantages and disadvantages

Method used

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  • Method for preparing o-methoxybenzaldehyde by use of micro-reaction device
  • Method for preparing o-methoxybenzaldehyde by use of micro-reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the microchannel reaction device, the diameter of the connecting pipe is 0.8mm, the length of the liquid inlet pipe is 15cm, the length of the connecting pipe between the T-valve and the microchannel reactor is 32cm, and the length of the connecting pipe between the microreactor and the outlet is 32cm; the volume of the microchannel reactor is 5ml.

[0029] Take 0.025mol (3.05g) of salicylaldehyde, add it to an aqueous solution containing 0.025mol sodium hydroxide and stir to form a homogeneous phase, and the volume of the mixed solution is 30mL; weigh 0.025mol (3.15g) of dimethyl sulfate, add THF to dilute to 30mL . The two materials are mixed and pumped into the microchannel reactor through the T-valve. The two reaction fluids flowed through the microreactor at 2.5mL / min respectively, the reaction molar ratio of salicylaldehyde and dimethyl sulfate was 1:1.0, the reactor temperature was 110°C, the reaction residence time was 1min, and the crude oil was collected a...

Embodiment 2

[0031] In the microchannel reaction device, the diameter of the connecting pipe is 2.0mm, the length of the inlet pipe is 15cm, the length of the connecting pipe between the T-shaped valve and the microchannel reactor is 32cm, and the length of the connecting pipe between the microreactor and the outlet is 32cm; the volume of the microchannel reactor is 2ml.

[0032] Take 0.025mol (3.05g) of salicylaldehyde, add it to an aqueous solution containing 0.0275mol sodium hydroxide and stir to form a homogeneous phase, and the volume of the mixed solution is 30mL; weigh 0.0275mol (3.47g) of dimethyl sulfate, add DMF to dilute to 30mL . The two materials are mixed and pumped into the microchannel reactor through the T-valve. The two reaction fluids flow through the microreactor at 0.1mL / min respectively, the molar ratio of salicylaldehyde and dimethyl sulfate is 1:1.1, the temperature of the reactor is 90°C, the reaction residence time is 10min, and the crude product is collected at ...

Embodiment 3

[0034] In the microchannel reaction device, the diameter of the connecting pipe is 1.0mm, the length of the inlet pipe is 15cm, the length of the connecting pipe between the T-valve and the microchannel reactor is 32cm, and the length of the connecting pipe between the microreactor and the outlet is 32cm; the volume of the microchannel reactor is 10ml.

[0035] Take 0.05mol (6.05g) of salicylaldehyde, add it to the aqueous solution containing 0.0525mol sodium hydroxide and stir to form a homogeneous phase, and the volume of the mixed solution is 40mL; weigh 0.065mol (8.19g) of dimethyl sulfate, add dioxane Dilute to 40mL. The two materials are mixed and pumped into the microchannel reactor through the T-valve. Two kinds of reaction solution fluids flowed through the microreactor at 2.5mL / min respectively, the reaction molar ratio of salicylaldehyde and dimethyl sulfate was 1:1.3, the temperature of the reactor was 70°C, the reaction residence time was 2min, and the crude oil ...

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Abstract

The invention discloses a method for preparing o-methoxybenzaldehyde by use of a micro-reaction device. The method comprises the following steps: dissolving salicylaldehyde into the aqueous solution of a strong base to obtain a homogeneous solution; dissolving dimethyl sulfate into an organic solvent to obtain a homogeneous solution; simultaneously pumping the two homogeneous solutions into the micro-reaction device, respectively, and reacting at a temperature within the range of 70-120 DEG C for 1-10 minutes; and collecting the liquid effluent, namely the crude product of o-methoxybenzaldehyde. The micro-reaction device has the characteristics of large specific surface area, high transfer rate, short contact time, low by-product, excellent heat transfer and mass transfer capacity, fast and direct amplification, high safety, good operability and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing o-methoxybenzaldehyde by utilizing a micro-reaction device. Background technique [0002] O-methoxybenzaldehyde, also known as fennel aldehyde, is an organic synthesis intermediate used in medicine, food and daily chemical industries. As a medium-flavored spice, it is widely used in the preparation of floral-flavored spices. It has a long-lasting hawthorn aroma. It is used as the main spice in hawthorn, sunflower, and lilac essences; it is used as a modifier in osmanthus essence; it can also be used in daily flavors and food. Essence, with essential oils such as tangerine, the effect is very good. In the pharmaceutical industry, it is used in the manufacture of antimicrobial drugs such as amoxicillin, and is an intermediate of antihistamines. As an excellent brightener for cyanide-free galvanizing DE additive, it can improve anodic ...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C47/575
CPCC07C45/64C07C47/575
Inventor 郭凯李昕陈安邦张锴
Owner NANJING UNIV OF TECH
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