Method of synthesizing 4H-pyran drug intermediate by catalyzing benzylidenemalononitrile derivative through immobilized enzyme
A technology of benzylidene malononitrile and immobilized enzyme is applied in the directions of biochemical equipment and methods, immobilization on or in inorganic carriers, chemical instruments and methods, etc., can solve problems such as no discovery, and achieve low cost , The preparation method is simple, and the repeated use performance is good.
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Embodiment 1
[0027] Step A:
[0028] Add 64mL deionized water and 8.2mL12mol·mL to the beaker -1 Concentrated hydrochloric acid, under the condition of slow stirring, add 2.0000g of cut block copolymer P123 and continue to stir. After the P123 is completely dissolved, raise the temperature to 45°C, and slowly add 4.4310g (0.0213mol) of normal Ethyl silicate, keep the dropping rate at 20 drops / min, and continue to stir and react for 24 hours after the dropping. The solution was transferred to a reaction kettle and crystallized at 140° C. for 48 hours. After crystallization, it was naturally cooled to room temperature, separated by suction filtration, washed three times with deionized water, then washed three times with absolute ethanol, and dried at room temperature to obtain a white solid powder. Finally, the obtained solid was calcined in a temperature-programmed muffle furnace at 550° C. for 6 hours to remove the template agent, and the heating rate was 5° C. / min to obtain the mesoporo...
Embodiment 2
[0032] Step A: Accurately weigh 1.0000g of triblock copolymer F127 at room temperature and add it to a 100mL polytetrafluoroethylene-lined autoclave, then add 38mL of deionized water and 1.38mL of 37% concentrated hydrochloric acid (12mol L -1 ), slowly stir to dissolve F127 completely, raise the temperature to 40°C, slowly add 4.2000g (0.0202mol) ethyl orthosilicate dropwise under vigorous stirring conditions, and keep the dropping rate at 20 drops / min. After the dropwise addition, it was stirred for 24 hours, and then the reaction kettle was placed at 100° C. for 24 hours of crystallization. After the crystallization, the reaction mixture was naturally cooled to room temperature, separated by suction filtration, washed three times with deionized water and then three times with absolute ethanol, and dried at room temperature for 12 hours to obtain a white solid powder. Finally, the obtained solid was calcined in a temperature-programmed muffle furnace at 550° C. for 6 h to re...
Embodiment 3
[0036] Step A: Accurately weigh 4.0003g of P123, add it to a mixture of 65mL deionized water and 10mL 37% concentrated hydrochloric acid, stir slowly until completely dissolved, raise the temperature to 40°C, add 1 dropwise under vigorous stirring conditions, 3,5-trimethylbenzene (TMB), keep the dropping rate at 20 drops / min. Control the mass ratio of TMB / P123 to 0.1, 0.3, 0.75 respectively, stir for 120min, then slowly add 8.5900g (0.0412mol) tetraethyl orthosilicate dropwise, also keep the dropping rate at 20 drops / min, mix well and let stand at constant temperature for 24h. Then add 5mL to dissolve 46.0020mg (0.0012mol) of NH 4 F aqueous solution, after rapid stirring, put it in the reaction kettle for crystallization reaction at 100°C for 24 hours. After the crystallization, cool to room temperature, separate by suction filtration, first wash three times with deionized water, then three times with absolute ethanol, and dry at room temperature A white solid powder was obta...
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