HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 70464278, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 13421116 | HCID 13421116 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Product | HCID 70464278 | HCID 70464278 | 70.7% |
Reaction Steps
A solution of 9-fluoro-11β-hydroxyandrosta-1,4-diene-3,17-dione (2.0 g) in a mixture of acetic anhydride (20 ml) and acetic acid (10 ml) containing p-toluenesulfonic acid (200 mg) is kept at room temperature for 40 hours. Sodium acetate (1.0 g) is added and the mixture is evaporated in vacuo. The residue is diluted with water and extracted with chloroform. The chloroform extracts are combined, washed with a dilute sodium bicarbonate solution and water, dried, evaporated and the residue is chromatographed on a column of silica gel to afford the title compound (1.6 g), melting point 229°-230° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04094840 |
| Source dataset | uspto-grants-1978_06 |
| ORD ID | ord-5303fca9da7643bdb81b999a2c24def7 |
| Source note | uspto-grants-1978_06 |