HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22931941, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 22931943 | HCID 22931943 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22931941 | HCID 22931941 | 30.4% |
Reaction Steps
Aluminum lithium hydride (1.62 g, 4.26 mmol) was dissolved in tetrahydrofuran (20 ml), followed by adding dropwise thereto 2-(1,3-dimethylbutyl)-4-pentafluoroethylaniline (974 mg, 3.3 mmol), and the resulting mixture was stirred at reflux temperature for 3 hours. Water was added to the reaction mixture in small portions under ice-cooling, followed by stirring for 10 minutes. Magnesium sulfate was added thereto and then stirred for 10 minutes. The reaction mixture was filtered through Celite and the filtrate was concentrated under reduced pressure, after which the residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to obtain 260 mg of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07459477B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-ab18b279681c4744b41059ad8229bc13 |
| Source note | uspto-grants-2008_12 |