Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22734139 | HCID 22734139 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22734480 | HCID 22734480 | 58.1% |
Reaction Steps
Under an argon atmosphere, a solution (7 ml) of Compound 46a (0.2 g) obtained in Step A in methylene chloride was cooled to −78° C., and then boron trifluoride ether complex (0.17 ml) and triethylsilane (0.33 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=20/1) to give Compound 46 (0.11 g, 58.1%) as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06716987B1 |
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| Source dataset | uspto-grants-2004_04 |
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| ORD ID | ord-4b61e0d4c66e4526a461242eac35aefd |
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| Source note | uspto-grants-2004_04 |
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