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Method for preparing 2-(2-oxo-2-phenethoxy) isobenzyl-1, 3-diketone

A technology of phenylethoxy and oxo, which is applied in the field of oxidative alkylation reaction to achieve the effect of simple process, mild reaction conditions, and no catalyst and oxidant participation

Inactive Publication Date: 2020-09-01
HUBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In recent years, researchers have mostly used metal catalyzed alkenes to obtain oxidative alkylation products, but there are few studies on the direct use of alkynes to obtain oxidative alkylation products

Method used

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  • Method for preparing 2-(2-oxo-2-phenethoxy) isobenzyl-1, 3-diketone

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Experimental program
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Embodiment 1

[0020] Add 0.2mmol of N-hydroxyphthalimide, 0.2mmol of phenylacetylene and magneton into the reactor, feed oxygen, and then add 2ml of 1,2-dichloroethane under oxygen atmosphere, and react The device was placed in an oil bath at 25°C to heat the reaction, the magnetic stirrer speed was adjusted to 400-600 rpm, and the reaction was carried out for 8-16 hours. After the reaction was completed, the reaction solution was transferred to a separatory funnel, dichloromethane and water were added for extraction, and the crude product obtained by vacuum distillation of the organic phase was collected. Finally, the crude product was subjected to column separation (ethyl acetate:petroleum ether=1:10) to obtain 2-(2-oxo-2-phenylethoxy)isobenzyl-1,3-dione as a white solid product.

[0021] The structure of the product is determined by H NMR and C NMR: 1 H NMR (400MHz, CDCl 3 )δ8.21(d,J=8Hz,2H),7.95-7.93(m,2H),7.84-7.82(m,2H),7.71(m,1H),7.55(t,J 1 =8Hz,J 2 =8Hz,2H). 13 CNMR (100MHz, CD...

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Abstract

The invention relates to a method for preparing 2-(2-oxo-2-phenylethoxy) isobenzyl-1, 3-diketone, which comprises the following steps: adding phenylacetylene and N-hydroxyphthalimide into a reactor, introducing oxygen into the reactor, adding 1, 2-dichloroethane, carrying out magnetic stirring, and putting the reactor into an oil bath pot to react; transferring the obtained reaction liquid into aseparating funnel, adding dichloromethane and water for extraction, and collecting a crude product of an organic phase after reduced pressure distillation; and carrying out column chromatography separation on the obtained crude product by adopting a system in which the ratio of ethyl acetate to petroleum ether is 1: 10, so as to obtain a white solid product of 2-(2-oxo-2-phenethoxy) isobenzyl-1, 3-diketone. The synthesis method has the advantages of mild reaction conditions, simple technological process, no participation of catalysts and oxidants and the like.

Description

technical field [0001] The invention relates to a method for the oxidative alkylation reaction of phenylacetylene and N-hydroxyphthalimide under the action of oxygen, in particular to the preparation of 2-(2-oxo-2-phenylethoxy)iso Benzyl-1,3-dione method. Background technique [0002] As an important class of organic synthesis reactions, oxidative alkylation reactions can not only synthesize multi-site reaction products cost-effectively in one step, but also convert starting materials into a variety of compounds with biological or pharmaceutical activities. [0003] In recent years, researchers have mostly used metal catalyzed alkenes to obtain oxidative alkylation products, but there are few studies on the direct use of alkynes to obtain oxidative alkylation products. Therefore, the present invention relates to an oxidative alkylation reaction of alkynes, which has no catalyst and additives, and can obtain oxidative alkylation products with a higher yield at room temperatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 张谦栗娟娟李家乐郝小松李栋
Owner HUBEI UNIV OF TECH
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