A chemical preparation method of icariside D2

Abstract

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a chemical preparation method of icariside D2, which comprises the following steps: (a) dissolving total acetyl-beta-glucose and a glycosylation acceptor in a solvent, adding a catalyst under protection of an inert atmosphere, and reacting under temperature rise until the reaction is complete to prepare an intermediate A; and (b) dissolving the intermediate A in a solvent, adding an alkaline catalyst, and stirring and reacting at room temperature to prepare icariside D2. The application efficiently completes the chemical synthesis of icariside D2 in large quantities through two reaction steps with commercially available total acetyl-beta-glucose as a starting material; the reaction condition is mild, the reaction yield is high, and the product purity is high.

Claims

1. A chemical preparation method for icariin D2, characterized in that, Includes the following steps: (a) Dissolve peracetyl-β-glucose and glycosylated receptor in a solvent, add a catalyst under an inert atmosphere, and heat the reaction until the reaction is complete to prepare intermediate A; the heating temperature is 45°C; the alcohol hydroxyl protecting group R in the glycosylated receptor is tert-butyldimethylsilyl; the catalyst is boron trifluoride ether. (b) Intermediate A was dissolved in a solvent, and an alkaline catalyst was added. The mixture was stirred at room temperature to prepare icariin D2.

2. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step a, the molar ratio of total acetyl-β-glucose to glycosylation receptor is 1.5-3:1, and the molar ratio of catalyst to glycosylation receptor is 1-10:

1.

3. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step a, the solvent is selected from one or more of anhydrous dichloromethane or anhydrous trichloromethane, and the inert atmosphere is one or more of nitrogen or argon.

4. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step b, the alkaline catalyst is selected from one or more of potassium carbonate, sodium carbonate, sodium methoxide, sodium ethoxide, sodium hydroxide, and potassium hydroxide.

5. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step b, the molar ratio of intermediate A to alkaline catalyst is 0.5-1:

1.

6. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step b, the solvent is selected from one or more of methanol, ethanol, tetrahydrofuran, acetonitrile, acetone, and water.

7. The chemical preparation method of icariin D2 as described in claim 1, characterized in that, In step b, the reaction time at room temperature is 0.5-1.5 h.

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