HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 22730842, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | Methyl 4'-formyl-2'-methoxy[1,1'-biphenyl]-4-carboxylate | HCID 11558086 | — |
| Catalyst | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22730842 | HCID 22730842 | — |
Reaction Steps
A suspension of methyltriphenylphosphonium bromide (785 mg, 2.2 mmoL) in THF (5 mL) was treated with 1M lithium bis(trimethylsilyl)amide in THF (2.2 mL), stirred for 30 minutes, treated with a solution of Example 122I (540 mg, 2.0 mmol) in THF (2 mL), stirred for 1 hour, and filtered through a pad of silica gel (20 g). The pad was rinsed with 1:1 ether/dichlormethane and concentrated. The concentrate was purified by flash column chromatography on silica gel with 20-50% dichloromethane/hexanes to provide the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06720338B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-3f49a387b08d4bff9a2a36ba4d9c0df4 |
| Source note | uspto-grants-2004_04 |