Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22734435 | HCID 22734435 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69543777 | HCID 69543777 | 56.7% |
Reaction Steps
Under an argon atmosphere, a solution of Compound 47a (0.4 g) obtained in Step A in methylene chloride (3 ml) was cooled to −78° C., and then boron trifluoride ether complex (0.3 ml) and triethylsilane (0.52 ml) were successively added thereto, followed by stirring at 0° C. for 2 hours. The reaction solution was poured into a saturated aqueous solution of sodium bicarbonate and the mixture was extracted with chloroform. The organic layer was washed with a saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=30/1) to give Compound 47 (0.27 g, 56.7%) as a yellowish brown oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06716987B1 |
|---|
| Source dataset | uspto-grants-2004_04 |
|---|
| ORD ID | ord-f707b7c5f8f3415495169e0fa6753824 |
|---|
| Source note | uspto-grants-2004_04 |
|---|