Forsythiasin sulfate and its derivatives, preparation method and application thereof
A technology of forsythiatin and its derivatives, which is applied in the fields of active ingredients of heterocyclic compounds, organic chemistry, antiviral agents, etc. It can solve the problems of easy oxidation, easy change of molecular configuration, instability of forsythiatin molecules, etc. problem, to achieve the effect of easy preparation method and high comprehensive yield
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Embodiment 1
[0035] 1. Add forsythiatin (4g, 10.75mmo) into 180ml of dry anhydrous pyridine, stir and dissolve to prepare forsythialine solution;
[0036] 2. Under ice-bath conditions, add dropwise a dichloromethane solution of chlorosulfonic acid (1.4ml, about 21.5mmol) in the forsythiatin solution, stir while adding, and the rate of addition is 1 drop (about 50ul / drop ) / 2s; That is, the mol ratio of forsythiatin and chlorosulfonic acid is 1:2 in the present embodiment.
[0037] 3. After the dropwise addition, raise the temperature under stirring and keep the temperature at 10°C to carry out the esterification reaction;
[0038] 4. The esterification reaction is complete under the condition that the temperature is maintained at 10°C. Add methanol solution (5ml) of sodium hydroxide after the reaction for 1h to adjust the pH value to 10, then distill the reaction mixture under reduced pressure to remove the solvent, and then load the sample on GF254 silica gel column chromatography, the el...
Embodiment 2
[0047] 1. Add forsythiatin (4g, 10.75mmo) into 180ml of dry anhydrous pyridine, stir and dissolve to prepare forsythialine solution;
[0048] 2. Under ice-bath conditions, add dropwise a dichloromethane solution of chlorosulfonic acid (1.4ml, about 21.5mmol) in the forsythiatin solution, stir while adding, and the rate of addition is 1 drop (about 50ul / drop ) / 2s; That is, the mol ratio of forsythiatin and chlorosulfonic acid is 1:2 in the present embodiment.
[0049] 3. After the dropwise addition, raise the temperature under stirring and keep the temperature at 10°C to carry out the esterification reaction;
[0050] 4. The esterification reaction was complete while keeping the temperature at 10°C. After 1 hour of reaction, methanol solution (5 ml) of potassium hydroxide was added to adjust the pH value to 10. Then, the reaction mixture was distilled off under reduced pressure to remove the solvent, and then loaded on GF254 silica gel column chromatography, the eluent is a mi...
Embodiment 3
[0059] 1. Add forsythiatin (4g, 10.75mmo) into 180ml of dry anhydrous pyridine, stir and dissolve to prepare forsythialine solution;
[0060] 2. Under ice-bath conditions, add dropwise a dichloromethane solution of chlorosulfonic acid (1.4ml, about 21.5mmol) in the forsythiatin solution, stir while adding, and the rate of addition is 1 drop (about 50ul / drop ) / 2s; That is, the mol ratio of forsythiatin and chlorosulfonic acid is 1:2 in the present embodiment.
[0061] 3. After the dropwise addition, raise the temperature under stirring and keep the temperature at 10°C to carry out the esterification reaction;
[0062] 4. The esterification reaction is complete while keeping the temperature at 10°C. After 1 hour of reaction, add ammonia water (5ml) to adjust the pH value to 8, then distill the reaction mixture under reduced pressure to remove the solvent, and then apply the sample to GF254 silica gel column chromatography , the eluent is a mixture of chloroform and methanol, wh...
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