Method for preparing symmetric diarylketone through catalytic oxidative carbonylation
A diaryl ketone, symmetrical technology, which is applied in the field of catalytic oxidative carbonylation to prepare symmetrical diaryl ketones, can solve the problems of high reaction temperature, high production cost, long reaction time and the like, and achieves simplified post-processing steps and reduced production cost. , the effect of mild reaction conditions
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1 2
[0023] The preparation of embodiment 1 benzophenone
[0024] Phenylboronic acid (0.249g, 2mmol), 5wt%Pd / CaCO 3 (0.0456g, Pd 0.01mmol) and CuI (0.0114g, 0.03mmol) were added to a 250mL PTFE-lined pressure reactor, then DMSO (10mL) was added, the reactor was installed, and slowly Air of 1.85 atm was introduced, and CO of 0.15 atm was introduced, and then the reactor was placed in an oil bath at 50° C. for 12 hours. After the reaction was stopped, the reaction kettle was cooled to room temperature, and the remaining gas in the kettle was slowly released in a fume hood. Open the reaction kettle, add 40 mL of ammonia water with a mass concentration of 5%, and filter and separate the palladium catalyst, which can be reused after being washed and dried. The mother liquor was extracted three times with dichloromethane (30mL), the organic phases were combined, and the organic phase was dried over anhydrous sodium sulfate, concentrated in vacuo to remove the solvent to obtain a crude ...
Embodiment 2～27
[0026] Different aryl boronic acids were used to prepare symmetrical diaryl ketones. The experimental operation was the same as in Example 1. The results are shown in Table 1.
[0027] Table 1 Different aryl boronic acids are used as raw materials to prepare diaryl ketones
[0028]
[0029]
[0030]
Embodiment 29
[0031] Embodiment 29 reclaims catalyst and prepares benzophenone
[0032] Phenylboronic acid (0.249g, 2mmol), recovered Pd / CaCO 3 Catalyst and CuI (0.0114g, 0.03mmol) were added in the pressure reactor of 250mL PTFE liner, then added DMSO (10mL), other operations were the same as Example 1, obtained benzophenone 0.169g, yield 93% , the product is a white solid. Separation and recovery of Pd / CaCO 3 The catalyst was used three more times, and the yields were 91%, 87% and 78%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More