HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 68126869, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 9-Fluoro-11-hydroxypregna-4,16-diene-3,20-dione | HCID 239405 | — |
| Catalyst | chromium (VI) trioxide | HCID 10219390 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68126869 | HCID 68126869 | — |
Reaction Steps
To a solution of 8.5 ml of dry pyridine in 220 ml of dry dichloromethane is added 5.1 g of chromium trioxide in small portions. When all the solid has dissolved, 25 g of dry Celite is added followed (with stirring) by a solution of 3.0 g of 9-fluoro-11β-hydroxypregna-4,16-diene-3,20-dione. The mixture is then stirred at room temperature for 30 minutes, filtered and the solids are washed with a small amount of dichloromethane. The filtrate and the washings are combined, washed with 5% hydrochloric acid, a dilute sodium bicarbonate solution and water, dried and evaporated to afford the product as a solid. One crystallization from acetone-hexane gives 2.65 g of the title compound, melting point 208°-211°C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03944584 |
| Source dataset | uspto-grants-1976_03 |
| ORD ID | ord-c78eca59f70c44ebba65167ca0ed1108 |
| Source note | uspto-grants-1976_03 |