Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 53688838 | HCID 53688838 | — |
| Solvent | Ammonia | HCID 222 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54130332 | HCID 54130332 | — |
Reaction Steps
To a blue solution of lithium metal (0.237 g, 34.2 mmol) in NH3 (1) (200 mL) at −78° C. was added a solution of 13-6 (2.60 g, 8.54 mmol) in THF (15 mL). The mixture was stirred for 15 minutes, then quenched by the addition of ammonium chloride until the blue color dispersed. An additional 30 mL of THF was added, and the mixture warmed to 35° C. to evaporate the ammonia. MgSO4 was added,the mixture was filtered through a celite pad. Following evaporative removal of the solvent, the residue was chromatographed (silica gel, 70:20:10 chloroform/ethyl acetate/MeOH) to give 13-7 as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06211184B1 |
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| Source dataset | uspto-grants-2001_04 |
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| ORD ID | ord-f87deeb136c544edb649bd684c4157b5 |
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| Source note | uspto-grants-2001_04 |
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