HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 17,17-Ethylenedioxy-2-methoxyestra-1,3,5(10)-trien-3-ol Acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 17,17-Ethylenedioxy-2-methoxyestra-1,3,5(10)-trien-3-ol | HCID 69736204 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 17,17-Ethylenedioxy-2-methoxyestra-1,3,5(10)-trien-3-ol Acetate | HCID 69736248 | 96.1% |
Reaction Steps
Under nitrogen, acetic anhydride (25 mL, 265 mmol) was added to a solution of the ketal (11) (4.5 g, 13.06 mmol) in dry pyridine (25 mL, 310 mmol). The reaction was stirred overnight at room temperature in the dark. After that time, methanol (50 mL) was added and solvents removed in vacuo. The treatment with methanol was repeated and the residue obtained crystallized from methanol to give the pure 3-acetate (12) (4.85 g, 96%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06852710B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-6df9962d8c7b408d88e338c40f53bfc4 |
| Source note | uspto-grants-2005_02 |