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Activating method of silicon dioxide and application thereof in catalyzing silicon cyanation of benzaldehyde

A silicon dioxide and formaldehyde silyl nitrile technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., to achieve mild reaction conditions, cheap and easy-to-obtain raw materials, and overcome difficulties in catalyst separation and recovery

Inactive Publication Date: 2012-03-14
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of silica for catalyzing the silylation of aldehydes has not been reported in the literature

Method used

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  • Activating method of silicon dioxide and application thereof in catalyzing silicon cyanation of benzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The silicon dioxide activated by the activation method of this embodiment was observed with a scanning electron microscope, and the scanning electron microscope picture of the activated silicon dioxide is shown in figure 1 . Depend on figure 1 It can be seen that the surface shape of the activated silica is regular, the particles are evenly dispersed, and there is no agglomeration.

[0020] Example 2

[0021] The method for activating silicon dioxide in this embodiment is as follows: 2 g of silicon dioxide is placed in a vacuum tube furnace, and the molecular pump unit is used to evacuate to 10 -2 Pa, the temperature was raised to 100° C. at a heating rate of 1° C. / min, and activated at a constant temperature for 12 hours. Other steps were the same as in Example 1 to obtain activated silica.

Embodiment 2

[0023] The method for activating silicon dioxide in this embodiment is as follows: 2 g of silicon dioxide is placed in a vacuum tube furnace, and the molecular pump unit is used to evacuate to 10 -2 Pa, the temperature was raised to 300° C. at a heating rate of 1° C. / min, and activated at a constant temperature for 12 hours. The other steps were the same as in Example 1 to obtain activated silica.

Embodiment 3

[0025] Adopt the application of the silica of embodiment 1 activation in benzaldehyde silyl nitrilation reaction, its using method is as follows:

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Abstract

The invention discloses an activating method of silicon dioxide, comprising the following steps of: adding silicon dioxide into a vacuum tubular furnace; vacuumizing to 10-20Pa by using a molecular pump unit; raising the temperature to 100-500DEG C at the temperature raising speed of 1DEG C / min; activating at constant temperature for 12 hours to obtain activated silicon dioxide; and sealing and preserving the activated silicon dioxide in an N2 atmosphere. The activating method of the silicon dioxide is simple and raw materials are low in prices and easily obtained. The activated silicon dioxide is used for catalyzing the silicon cyanation of benzaldehyde without adding other assistants, the reaction condition is mild and the yield is high; a catalyst is separated from a product by simple filter, so the invention overcomes the technical problem that the catalyst is difficult to separate in the silicon cyanation; and in addition, the catalyst can be recycled and still has high catalyticactivity after being used for 4 times. The activated silicon dioxide can be used for catalyzing the silicon cyanation of other aldehyde substances.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to the activation of silicon dioxide and its application in catalyzing the silylation reaction of benzaldehyde. Background technique [0002] Silicon nitrilation is one of the most important reactions for forming C–C bonds in organic synthesis. The cyanohydrin obtained by the silylation reaction is an important intermediate for the synthesis of some multifunctional compounds, and the chiral cyanohydrin obtained by the asymmetric silylation reaction is one of the important chiral sources in the asymmetric synthesis. Its A series of optically pure chiral compounds can be synthesized through multi-step conversion of two functional groups. At the same time, cyanohydrins are also the starting materials for the synthesis of many drugs and important constituent fragments of some natural products and pesticides. [0003] Catalytic silicon nitrilation reaction of aldehyde ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18B01J21/08
CPCY02P20/584
Inventor 高子伟代景丽李亚妮徐伟李金灵
Owner SHAANXI NORMAL UNIV