HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 67364108, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl orthoformate | HCID 31214 | — |
| Reactant | HCID 67361589 | HCID 67361589 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67364108 | HCID 67364108 | 78% |
Reaction Steps
Triethyl orthoformate (2 ml, 12 mmol) and p-Toluenesulfonic acid (20 mg, 0.10 mmol) were added to a suspension of 15α-acetoxy-18-methyl-estr-4-en-3,17-dione (2 g, 5.81 mmol) in ethanol (20 ml). The mixture was stirred at room temperature for 1 h. Potassium carbonate (1.1 g, 8.06 mmol) in solution in water (20 ml) was added and the mixture was heated under reflux for 2 h, cooled to 10° C. and water (20 ml) was then added. The precipitate was filtered, washed with water and dried under vacuum, to afford 3-ethoxy-18-methyl-estra-3,5,15-trien-17-one (1.3 g, yield: 78%). mp and 1H-NMR were in accordance with those obtained for example 2. HPLC analysis was as shown in FIG. 1b.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09012667B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-4923c750e02747e496387192df33c89a |
| Source note | uspto-grants-2015_04 |