Method for preparing celecoxib oxide
A technology of celecoxib and oxides, which is applied in the field of simple preparation of celecoxib oxides, can solve the problems of numerous reaction steps, affecting the reaction yield, cumbersome operation, etc., achieves good purification effect, simplifies experimental steps, The effect of experimenting with simplicity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0035] Dissolve 25 mg (0.1 mmol) of copper sulfate pentahydrate and 81.1 mg (0.3 mmol) of potassium persulfate in 2 ml of water to obtain a blue mixed solution; then heat the mixed solution to 65 ° C; then add 38.1 mg (0.1 mmol) of celecoxib ) was dissolved in 1ml of acetonitrile solvent and added to the mixed solution to obtain a light green solution, and the light green solution was heated to condense and reflux for 45 minutes; the passing specification was The thin-layer chromatographic plate of F-254 traces whether the reaction is completed. After the reaction is over, add 2ml of water and 6ml of dichloromethane to the reaction solution for extraction. The extract of the lower layer is spin-dried with dichloromethane, and then add anhydrous Dry over sodium sulfate to remove water, filter and take the filtrate, finally add silica gel powder and spin dry dichloromethane, purify the product by column chromatography, spin dry the solvent again, and vacuumize to obtain celecoxi...
Embodiment 2
[0038] Dissolve 25 mg (0.1 mmol) of copper sulfate pentahydrate and 47.4 mg (0.3 mmol) of potassium persulfate in 2 ml of water to obtain a blue mixed solution; then heat the mixed solution to 65 ° C; then add 38.1 mg (0.1 mmol) of celecoxib ) was dissolved in 1ml of N,N-dimethylformamide solvent and added to the mixed solution to obtain a light green solution, and the light green solution was heated to condense and reflux for 45min; after the reaction was completed, 2ml of water and 6ml of dichloromethane were added to the reaction solution Extraction, take the extract of the lower layer and spin dry the dichloromethane, add anhydrous sodium sulfate to dry and remove water, filter and take the filtrate, finally add silica gel powder and spin dry the dichloromethane, purify the product by column chromatography, spin again Dry the solvent and vacuumize to obtain 20.5 mg of celecoxib oxide with a yield of 52%.
Embodiment 3
[0040] Dissolve 25 mg (0.1 mmol) of copper sulfate pentahydrate and 81.1 mg (0.3 mmol) of potassium persulfate in 2 ml of water to obtain a blue mixed solution; then heat the mixed solution to 65 ° C; then add 38.1 mg (0.1 mmol) of celecoxib ) was dissolved in 1ml dimethyl sulfoxide solvent and added to the mixed solution to obtain a light green solution, and the light green solution was heated to condense and reflux for 45min; The extract was spin-dried in dichloromethane, then dried with anhydrous sodium sulfate to remove water, filtered and the filtrate was taken, and finally silica gel powder was added to spin-dry dichloromethane, the product was purified by column chromatography, the solvent was spin-dried again, and vacuumized 22.5 mg of celecoxib oxide was obtained, with a yield of 57%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More