HuagongsheHuagongshe Chemistry Print Report · For research reference only
MAGNESIUM SILICATE (synthetic) → 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-20-oxopregna-5,7,16-triene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | MAGNESIUM SILICATE (synthetic) | HCID 61680 | — |
| Reactant | Cornforth reagent | HCID 2724130 | — |
| Reactant | 1alpha,3beta-bis(tert-butyldimethylsilyloxy)-20(S)-hydroxypregna-5,7,16-triene | HCID 12020078 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-20-oxopregna-5,7,16-triene | HCID 12020082 | 57.6% |
Reaction Steps
A suspension of 1α,3β-bis(tert-butyldimethylsilyloxy)-20(S)-hydroxypregna-5,7,16-triene (600 mg, 1.07 mmol), pyridinium dichromate (610 mg, 1.61 mmol) and Florisil (3 g) in dichloromethane (10 ml) was stirred at room temperature for 1.5 hours, then ultrasonicated for 2.5 hours. The solvent was distilled off under reduced pressure and the resulting residue was diluted with diethyl ether and filtered through Celite. The solvent was distilled off under reduced pressure and the resulting residue was purified by column chromatography (hexane:ethyl acetate=15:1) to give the title compound as a colorless solid (343 mg, 57%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06184398B2 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-66b816cb1bd8449781b815c0faef2115 |
| Source note | uspto-grants-2001_02 |