A kind of preparation method of sancycline
A sancycline and environmental technology, applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problems of inapplicability to industrial production, cumbersome post-processing, low reaction yield, etc., to facilitate purification , good product purity and high product yield
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Embodiment 1
[0032] Add 20g of aureomycin to 150ml of methanol, stir, and add 25g of sulfuric acid dropwise in an ice-water bath. Add 0.5g of 5% rhodium on carbon catalyst, vacuum suction into 500ml autoclave. After nitrogen replacement three times, hydrogen was introduced, and the hydrogen pressure was controlled at 1.5-2.5 MPa. The hydrogenation reaction was carried out at room temperature for 24 hours. The reaction liquid was detected by HPLC.
[0033] Release the hydrogen pressure and replace with nitrogen three times. Blowing, filtering, 20ml methanol washing filter cake, reclaiming filter cake rhodium carbon catalyst. The filtrate was concentrated under reduced pressure, and the concentration temperature did not exceed 30°C. The concentrate was dissolved in 200ml deionized water.
[0034] Pack 600ml of XAD1600 macroporous adsorption resin into the column. After pretreatment, wash the resin with 300ml of deionized water. After putting the above-mentioned treated solution on the co...
Embodiment 2
[0036] Add 20 g of demethylaureomycin to 200 ml of ethanol, stir, and add 30 g of perchloric acid dropwise in an ice-water bath. Add 0.6g of 5% rhodium on carbon catalyst, vacuum suction into 500ml autoclave. After nitrogen replacement three times, hydrogen was introduced, and the hydrogen pressure was controlled at 2-2.5 MPa. The hydrogenation reaction was carried out at room temperature for 22 hours. The reaction liquid was detected by HPLC.
[0037] Release the hydrogen pressure and replace with nitrogen three times. Blowing, filtering, 20ml ethanol washing filter cake, reclaims filter cake rhodium carbon catalyst. The filtrate was concentrated under reduced pressure, and the concentration temperature did not exceed 30°C. The concentrate was dissolved in 200ml deionized water.
[0038]Pack 700ml of XAD1800 macroporous adsorption resin into the column. After pretreatment, wash the resin with 400ml of deionized water. After putting the above-mentioned treated solution on ...
Embodiment 3
[0040] Add 20g of demethyltetracycline to 150ml of methanol, add 35g of methanesulfonic acid, and stir to dissolve. Add 0.8g of 5% rhodium on carbon catalyst, vacuum suction into 500ml autoclave. After nitrogen replacement three times, hydrogen was introduced, and the hydrogen pressure was controlled at 1.5-2.5 MPa. The hydrogenation reaction was carried out at room temperature for 18 hours. The reaction solution was detected by HPLC.
[0041] Release the hydrogen pressure and replace with nitrogen three times. Blowing, filtering, 20ml methanol washing filter cake, reclaiming filter cake rhodium carbon catalyst. The filtrate was concentrated under reduced pressure, and the concentration temperature did not exceed 30°C. The concentrate was dissolved in 200ml deionized water.
[0042] Pack 600ml of XAD2000 macroporous adsorption resin into the column. After pretreatment, wash the resin with 400ml of deionized water. After putting the above-mentioned treated solution on the c...
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