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Preparation method of propofol and structural analogues of propofol

A compound, isopropyl technology, applied in the field of preparation of propofol and its structural analogs, can solve the problems of dangerous hydrogenation conditions, acid corrosion, complicated reaction operation and the like

Active Publication Date: 2017-04-26
李宏 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction principle is the same as the US patent, and there are also problems such as complicated reaction operation, severe acid corrosion, and dangerous hydrogenation conditions.

Method used

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  • Preparation method of propofol and structural analogues of propofol
  • Preparation method of propofol and structural analogues of propofol
  • Preparation method of propofol and structural analogues of propofol

Examples

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Effect test

preparation example Construction

[0071] The preparation method of solid acid described below comprises: 90% (volume fraction) vitriol oil and 20% (volume fraction) phosphoric acid are mixed by volume ratio 5:1 and mixed acid is made; 120 mesh gacs are mixed with above-mentioned mixed acid by weight 10: 1. Mix evenly, soak for 10 hours and put it into muffle furnace for carbonization for 2 hours. The carbonization temperature is 450-500°C. The obtained solid is sulfonated with 98% (volume fraction) concentrated sulfuric acid for 8 hours, and dried until the water content is less than 10%, to obtain the solid acid catalyst.

[0072] The distillation method described below includes: first use a Roots pump to distill low-boiling substances at a temperature of 50-60°C and a vacuum of -0.05-0.09MPa, then rectify with a packed column at a vacuum of 1-100Pa and the rectification temperature For 110 ~ 140 ° C, collect the corresponding fractions.

Embodiment 1

[0073] Example 1 Preparation of 2,6-dimethylphenol

[0074] (1) In a 500ml reaction flask, add 138g (1mol) of p-hydroxybenzoic acid, 160g (5mol) of methanol, and 50g of solid acid, and stir until the solid is uniform. Put it into an ultrasonic reactor, install a reflux device, set the reaction temperature to 40-60°C, ultrasonic power to 500W, and react for 1-3 hours. The reaction solution gradually changes from white to yellow, and then to orange-red. Use HPLC to track the reaction conversion rate, the reaction is complete until the p-hydroxybenzoic acid is less than 5%, stop the reaction, filter out the solid acid catalyst, the catalyst can be used for the next reaction; the filtrate is placed at about 5-10°C for crystallization for 6-10 hours The crystals were filtered, dried at 50-60°C for 6 hours, detected by HPLC, the impurity was less than 0.1%, and 141 g of intermediate 4-hydroxy-3,5-dimethylbenzoic acid was obtained with a yield of 85%.

[0075] Above-mentioned step (...

Embodiment 2

[0089] Example 2 Preparation of 2,6-di-ethylphenol

[0090](1) In a 500ml reaction flask, add 138g (1mol) of p-hydroxybenzoic acid, 230g (5mol) of ethanol, and 50g of solid acid, and stir until the solid is uniform. Put it into an ultrasonic reactor, install a reflux device, set the reaction temperature to 40-60°C, ultrasonic power to 500W, and react for 1-3 hours. The reaction solution gradually changes from white to yellow, and then to orange-red. Adopt HPLC (method is the same as embodiment 1) tracking reaction conversion rate, react to p-hydroxybenzoic acid less than 5% and calculate reaction completely, stop reaction, filter out solid acid catalyst, catalyzer can apply mechanically next time to react; Filtrate is placed about 5 Crystallized at ~10°C for 6-10 hours, filtered the crystals, dried at 50-60°C for 6 hours, detected by HPLC, the impurities were less than 0.1%, and 155g of intermediate 4-hydroxy-3,5-diethylbenzoic acid was obtained, with a yield of 80% .

[009...

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Abstract

The invention relates to a preparation method of propofol and structural analogues of propofol. The preparation method comprises the steps as follows: preparing an intermediate from p-hydroxybenzoic acid and alkyl alcohol as raw materials under the action of a solid acid catalyst, and then preparing a target product by a decarboxylase reaction. The preparation method has the characteristics of being green in synthesis, realizing biotransformation, causing little pollution, producing few by-products and the like, and is suitable for industrial production; the purity of the prepared products such as propofol is 99.6% or higher, which meets various medicinal standards.

Description

technical field [0001] The invention relates to a preparation method of propofol and structural analogues thereof. Background technique [0002] Alkylphenols are a class of specific aromatic products that are substituted on the 2 and 6 positions of phenol, and are widely used in pharmaceutical and chemical industries. Propofol (trade name: Propofol, Propofol, Diprivan), whose chemical name is 2,6-diisopropylphenol, is a rapid and short-acting intravenous anesthetic of alkylphenols widely used clinically. It activates the GABA receptor-chloride complex , play a sedative and hypnotic effect. It has rapid onset, short action time, quick and complete recovery, few adverse reactions, no sequelae, low incidence of postoperative nausea and vomiting, wide application range (can be used for anesthesia induction, maintenance and auxiliary epidural anesthesia), easy to control dosage and other excellent characteristics. Since its anesthetic activity was discovered in 1977, it has be...

Claims

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Application Information

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IPC IPC(8): C07C37/50C07C39/07C07C39/06C07C51/353C07C65/03B01J27/053C12N9/88G01N30/02C12P7/22
CPCB01J27/053C07C37/50C07C51/353C12N9/88C12P7/22C12Y401/01G01N30/02C07C39/06C07C39/07C07C65/03
Inventor 潘自国李宏郑方军张金涛陈静芳范玲玲
Owner 李宏
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