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Method for preparing benzil by iron-catalyzed air oxidation of benzoin

A technology for oxidizing benzene and benzil, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc. Wide range, easy product solvent separation, no storage leakage effect

Inactive Publication Date: 2018-07-13
ZHEJIANG WANLI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN 102476063 B discloses a bifunctional catalyst and its application in the preparation of benzil by dehydrogenation / oxidation of benzoin. Anion / cation exchange resin is used to load and bind a catalyst of variable valence metal or transition metal element to catalyze the dehydrogenation of molecular oxygen Hydrogen / benzoin oxide prepares benzil, the conversion rate of raw materials is high, and the separation and recovery of catalyst is simple and convenient, but the preparation of catalyst is relatively complicated; CN103755536 A discloses a method of using silica gel GF254 to immobilize benzoin, and air oxidation under heating to prepare benzil The method is low in cost and high in yield, but there are many operations and post-processing steps

Method used

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  • Method for preparing benzil by iron-catalyzed air oxidation of benzoin

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Embodiment 1

[0023] Build a reflux reaction device on a constant temperature water bath, adjust the reaction temperature to 80°C, adjust the hydrogen ion concentration to about 0.7mol / L with 33mL dimethyl sulfoxide (DMSO) with hydrochloric acid, add 2.1g benzoin and 0.2g catalyst FeNO 3 9H 2 O, reacted for 60min, after the reaction was finished, the reaction solution was poured into a beaker, after cooling to room temperature, an equal volume of distilled water was added, and after standing in an ice-water bath to precipitate solids, vacuum filtration was carried out, and the dried crude product was analyzed by high performance liquid chromatography for benzil The conversion rate reached 85.6%, and the crude ethanol was recrystallized to obtain yellow needle-like crystals with a measured melting point (mp) of 94.2-96.0°C.

Embodiment 2

[0025] Set up a reflux reaction device in an ultrasonic reactor, adjust the reaction temperature to 80°C, adjust the hydrogen ion concentration to about 1.2mol / L with 33mL dimethyl sulfoxide (DMSO) with hydrochloric acid, and add 2.1g benzoin and 0.2g catalyst FeNO 3 9H 2O, ultrasonic power 180W, reaction 60min, after the reaction, pour the reaction solution into a beaker, add an equal volume of distilled water after cooling to room temperature, leave it in an ice-water bath to precipitate solids, and carry out vacuum suction filtration, and dry the crude product by high performance liquid chromatography Analysis of benzil conversion rate reached 95.24%, good repeatability of synthetic reaction, RSD reached 0.57% (n=3), crude ethanol recrystallization obtained yellow needle-like crystals, measured melting point (mp) was 94.4-95.6 ° C, infrared spectrum ( FT-IR), ultraviolet-visible spectroscopy (UV-Vis), high-performance liquid chromatography-mass spectrometry coupled with ext...

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Abstract

The invention discloses a method for preparing benzil by iron-catalyzed air oxidation of benzoin. The method comprises the following steps: taking acidified dimethyl sulfoxide (DMSO) as a solvent, adopting iron salt containing iron ions as a catalyst under the heating condition and oxidizing the benzoin under the action of an oxidant to prepare benzyl; the reaction temperature under the heating condition is 40-80 DEG C; the oxidant comprises atmospheric air, high oxygenated air and oxygen. The method disclosed by the invention is mild in reaction condition, green and clean, and a product solvent is easy to separate.

Description

technical field [0001] The invention relates to the field of organic chemistry and organic synthesis, in particular to a method for preparing benzil by iron-catalyzed air oxidation of benzoin. Background technique [0002] Benzoin, CAS number 119-53-9, also known as benzoin, α-hydroxy-α-phenylacetophenone, α-hydroxyphenyl phenyl ketone, 2-hydroxy-2-phenylacetophenone, benzene Formylbenzyl alcohol, 2-hydroxy-1,2-diphenylethanone, is a colorless or white crystal, the shape is irregular small pieces, slightly flat, often bonded into agglomerates; the texture is brittle, easy to Crushed, the cross-section is flat and white, and gradually turns light yellow-brown to reddish-brown after being placed; it softens and melts when heated; the smell is fragrant, the taste is slightly pungent, and it has a gritty feeling when chewed. [0003] Beniloyl, CAS No. 134-81-6, also known as dibenzoyl, dibenzoyl, dibenzoyl, diphenyl ketone, yellow prismatic crystalline powder, used for organic ...

Claims

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Application Information

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IPC IPC(8): C07C45/39C07C49/784
CPCC07C45/39C07C49/784
Inventor 张凯龙陈倩婷胡怡超
Owner ZHEJIANG WANLI UNIV
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