The refining method of acetyl dehydroepiandrosterone enol trifluoromethanesulfonate
A technology of epiandrosterone enol trifluoromethanesulfonate and a refining method, which is applied in the field of medicine, can solve problems such as lack of refining, achieve the effects of simple and practical operation, and reduce difficulty and production cost
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
example 1
[0060] S1: 10 g of triflate oil concentrate with a purity of 45% was extracted six times with 100 mL of n-hexane, and the extracts were combined;
[0061] S2: Rotary evaporation recovers n-hexane, and the residue is about 7.5g, which is the product after one refinement. Dissolve the refined acetyl dehydroepiandrosterone triflate in ethanol and heat it at about 50°C form a saturated solution;
[0062] S3: maintaining the temperature in step S2, slowly adding 50% formic acid to supersaturation to form a supersaturated solution;
[0063] S4: naturally cooling to room temperature, a solid product is precipitated; the solid is crystal-grown and filtered to obtain a filtrate and a solid, respectively, and the solid is the first part of acetyl dehydroepiandrosterone enol triflate;
[0064] S5: transfer the filtrate in step S4 to another crystallization bottle, and then slowly add 50% formic acid until the solution becomes turbid to form a supersaturated solution;
[0065] S6: Place...
example 2
[0069] S1: 10 g of triflate oily concentrate with a purity of 45% was extracted six times with 100 mL of petroleum ether (temperature between 60 and 90° C.), and the extracts were combined;
[0070] S2: Petroleum ether was recovered by rotary evaporation, and the residue was about 7.8g, which was the product after the first refinement. The acetyl dehydroepiandrosterone trifluoromethanesulfonate after the first refinement was dissolved in dichloromethane, and refluxed temperature to form a saturated solution;
[0071] S3: maintaining the temperature in step S2, slowly adding 80% formic acid to supersaturation to form a supersaturated solution;
[0072] S4: naturally cooling to room temperature, a solid product is precipitated; the solid is crystal-grown and filtered to obtain a filtrate and a solid, respectively, and the solid is the first part of acetyl dehydroepiandrosterone enol triflate;
[0073] S5: transfer the filtrate in step S4 to another crystallization bottle, and t...
example 3
[0078] S1: 10 g of triflate oil concentrate with a purity of 49% was extracted 6 times with 100 mL of cyclohexane, and the extracts were combined;
[0079] S2: Cyclohexane is recovered by rotary evaporation, and the residue is about 7.0g, which is the product after the first refinement; the acetyl dehydroepiandrosterone trifluoromethanesulfonate after the first refinement is dissolved in 80% methanol, and A saturated solution is formed at 50°C;
[0080] S3: maintaining the temperature in step S2, slowly adding 50% methanol to supersaturation to form a supersaturated solution;
[0081] S4: naturally cooling to room temperature, a solid product is precipitated; the solid is crystal-grown and filtered to obtain a filtrate and a solid, respectively, and the solid is the first part of acetyl dehydroepiandrosterone enol triflate;
[0082] S5: transfer the filtrate in step S4 to another crystallization bottle, and then slowly add 50% methanol until the solution becomes cloudy to for...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More