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Method for preparing ethyl vanillin from sassafras oil

A technology of ethyl vanillin and sassafras oil, which is applied in the field of preparing ethyl vanillin from sassafras oil, can solve the problems of difficult product purification, urgent improvement of yield, and long reaction cycle, and achieves mild process conditions and improved Utilization rate, the effect of less usage

Pending Publication Date: 2020-07-03
绵阳三香汇生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ethyl wood phenol-chloral method has high yield and low pollution, but the reaction cycle is long, the cost of raw materials is high, and product purification is difficult, so it is rarely used in industry
Synthesis of ethyl vanillin by ethyl xylol-glyoxylic acid method has been recognized by the same industry at home and abroad, but its yield still needs to be improved urgently

Method used

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  • Method for preparing ethyl vanillin from sassafras oil

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Embodiment 1

[0030] Embodiment 1 sassafras oil prepares ethyl vanillin

[0031] 1. Raw materials: sassafras oil, KOH, methanol, diethyl sulfate, ethanol, sulfuric acid, acetic anhydride, sodium carbonate, ozone, sodium pyrosulfite, liquid caustic soda, concentrated hydrochloric acid

[0032] 2. Preparation process:

[0033] (1) Put 100g of sassafras oil, 100g of methanol, and 100g of potassium hydroxide into the reaction flask, raise the temperature to 130°C for 1 hour, then distill methanol under normal pressure, and raise the temperature while steaming methanol until the temperature reaches 150- Between 160°C, the duration is about 6h. Wait until the content of safrole <1%, that is judged as the end of the reaction, stop heating. When the reaction solution is cooled to 90°C, slowly add 200g of water and mix well. Then the reaction solution was poured into a separatory funnel, allowed to stand for phase separation, and the lower alkali aqueous phase was separated, and 320 g of the uppe...

Embodiment 2

[0039] The preparation of embodiment 2 ethyl vanillin

[0040] 1. Raw materials: sassafras oil, KOH, methanol, diethyl sulfate, ethanol, sulfuric acid, acetic anhydride, sodium carbonate, ozone, sodium pyrosulfite, liquid caustic soda, concentrated hydrochloric acid

[0041] 2. Preparation process:

[0042] (1) Put 500g of sassafras oil, 400g of methanol, and 400g of potassium hydroxide into a reaction flask, raise the temperature to 120-140°C for 1 hour, then distill out methanol under normal pressure, and raise the temperature while distilling methanol until the temperature reaches Between 150-160°C, the duration is about 6h. Wait until the content of safrole <1%, that is judged as the end of the reaction, stop heating. When the reaction liquid is cooled to 90°C, slowly add 800g of water and mix well. Then the reaction solution is poured into a separatory funnel, left to separate phases, the lower alkali aqueous phase is separated, and 1500 g of the upper layer potassium ph...

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Abstract

The invention discloses a method for preparing ethyl vanillin from sassafras oil. The method comprises the following steps: (1) subjecting sassafras oil, methanol and potassium hydroxide to mixing andreacting, carrying out cooling and phase splitting, and collecting a phenol potassium salt solution at an upper layer; (2) subjecting the phenol potassium salt solution and diethyl sulfate to mixingand reacting, performing phase splitting, and collecting an upper-layer solution, namely mixed ether; (3) subjecting the mixed ether, ethanol, water and concentrated sulfuric acid to mixing and reacting, and carrying out cooling, filtering and recrystallizing to obtain concentrated vanillin; (4) mixing acetic anhydride and sodium carbonate, dropwise adding isoeugenol for a reaction, and carrying out condensing, refluxing and distilling to obtain isoeugenol acetate; (5) mixing isoeugenol acetate, ethanol and water, introducing ozone-containing oxygen flow for a reaction, adding an aqueous solution of sodium metabisulfite, and recovering ethanol to obtain acetyl ethyl vanillin; and (6) subjecting acetyl ethyl vanillin, methanol, concentrated hydrochloric acid and water to mixing and reacting, recovering methanol, separating oil and water phases, and then successively carrying out washing, reduced-pressure rectifying and recrystallizing to obtain ethyl vanillin.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for preparing ethyl vanillin from sassafras oil. Background technique [0002] Ethyl vanillin, also known as ethyl vanillin, chemical name is 3-ethoxy-4-hydroxybenzaldehyde, white to light yellow needle crystal, melting point 77-78 ℃, slightly soluble in water, soluble in ethanol. It has the aroma of sweet chocolate and all the aroma of vanillin. It has the characteristics of pure and elegant fragrance, less usage, sufficient fragrance and no discoloration. It is widely used in spices, cosmetics, food additives, medicine and other industries. It has not been found in natural products, and it is mainly synthesized by chemical methods. [0003] A variety of different synthetic routes have been developed for ethyl vanillin, mainly p-hydroxybenzaldehyde method and ethyl wood phenol-glyoxylic acid method. The technical route of synthesizing ethyl vanillin with p-h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/64C07C47/575
CPCC07C45/64C07C47/575
Inventor 张焜周锦李良龙李波曾林久熊智朱强
Owner 绵阳三香汇生物科技有限公司
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