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Oxidative coupling method for preparing kilogram-grade novel biphenol and catalyst thereof

A technology of biphenyltetraphenol and oxidative coupling, which is applied in the field of oxidative coupling and catalysts for the preparation of kilogram-level new biphenyltetraphenols, and can solve the problems of increasing reaction steps and experimental procedures

Active Publication Date: 2020-11-10
广东欧凯新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, halogenated hydrocarbons need to be prepared in advance, which increases the reaction steps and experimental procedures.

Method used

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  • Oxidative coupling method for preparing kilogram-grade novel biphenol and catalyst thereof
  • Oxidative coupling method for preparing kilogram-grade novel biphenol and catalyst thereof
  • Oxidative coupling method for preparing kilogram-grade novel biphenol and catalyst thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Acidic system preparation method

[0017] In the kilogram-level synthetic ventilation room, a 10L double-layer glass jacketed reactor is equipped with explosion-proof mechanical stirring paddles, dropping funnels, explosion-proof high and low temperature cycles, temperature probes, reflux condensers, and discharge valves. Add 4,6-di-tert-butylresorcinol (4.5mol), acidic solution (3.8L), stir until dissolved, then drop a quantitative amount of metal oxidant (0.45–6.75mol) and water into the reaction kettle Clear solution (2L). During the dropwise addition, the reaction kettle has a partial exothermic phenomenon, and an explosion-proof high and low temperature cycle is required to control the temperature in the kettle. After the dropwise addition, stir and react at the rated temperature (-20-50°C) for 1-12 hours. After the reaction is completed, when a large amount of solid particles are precipitated in the kettle, the filter cake obtained by filtering in batches with ...

Embodiment 2

[0022] Alkaline system preparation method

[0023] In the kilogram-level synthetic ventilation room, a 10L double-layer glass folder is equipped with explosion-proof mechanical stirring paddles, dropping funnels, explosion-proof high and low temperature cycles, temperature probes, gas conduits, reflux condensers, and discharge valves. Add part of the reaction solvent (3L), basic compound (0.0225-0.9mol) and quantitative metal compound agent (0.0225-0.45mol) into the reaction kettle in sequence, and stir evenly at room temperature for 0.5-1 hour; during stirring, Continuously feed oxygen or compressed air below the reaction liquid level (distinguishable by bubbling). After the metal-organic base complex is formed, slowly drop the dissolved 4,6-di-tert-butylresorcinol solution (4.5mol, 3.8L) into the reactor with a dropping funnel, and keep it flowing. into oxygen or air. After the dropwise addition, the reaction solution was stirred and reacted at a rated temperature (25-40...

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Abstract

The invention discloses an oxidative coupling synthesis method for preparing novel biphenol and a catalyst thereof. The novel biphenol has a structure as shown in a general formula I which is described in the specification. Under the action of metal compounds such as copper, iron, nickel, manganese, cobalt, chromium, magnesium, sodium, potassium and the like, metal complexes or basic metal complexes and an acid solution or an oxygen-containing organic alkaline solution, alkoxy benzene, alkylphenol or alkoxy phenol carbon-carbon bond oxidative coupling reaction is performed to obtain a compoundshown in general formula I; the invention discloses an oxidative coupling preparation method of novel biphenol and catalyst screening.

Description

technical field [0001] The invention relates to an oxidative coupling method for preparing kilogram-level novel biphenyltetraphenols and a catalyst thereof, including oxidative coupling conditions and catalyst screening. Background technique [0002] Coupling reaction is a process in which two organic chemical units perform a certain chemical reaction to obtain an organic molecule, including free radical coupling reaction and transition metal catalyzed coupling reaction. Classical coupling reactions such as Suzuki, Heck, Sonogashira, Stille, Kumada, Negishi, and Hiyama are coupling reactions between organometallic reagents and preactivated halohydrocarbons. However, halogenated hydrocarbons need to be prepared in advance, which increases the reaction steps and experimental procedures. In addition, the coordination compound of noble metal palladium Pd(PPh 3 ) 4 is the most commonly used catalyst for this type of reaction, other catalysts include PdCl 2 (PPh 3 ) 2 , PdCl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C39/15B01J23/34B01J23/26B01J27/02B01J27/128B01J27/06B01J27/122B01J27/055B01J31/02B01J31/22B01J31/18
CPCC07C37/11B01J27/122B01J27/055B01J31/1805B01J31/2213B01J2231/4205B01J31/0227B01J31/1815B01J27/26B01J2531/16B01J2531/845C07C39/15Y02P20/52
Inventor 张润通彭江华
Owner 广东欧凯新材料有限公司