HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 54417824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 11623143 | HCID 11623143 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54417824 | HCID 54417824 | — |
Reaction Steps
5.0 g (18.6 mmol) 4-(1,3-dioxo-1H,3H-benzo[de]isoquinolin-2-yl)-butylamine are dissolved in 200 ml THF and 6.1 g (160.7 mmol) LiAlH4 are added in portions under cooling. The suspension is stirred for 24 hours at RT and for 8 hours under reflux. After cooling, ethanol is carefully added dropwise until no more foam appears. The mixture is filtered and the filtrate is concentrated under vacuum. The residue is distributed between chloroform and water. The organic phase is dried over sodium sulfate and, after withdraw of the solvent, chromatographically purified over silica gel with CHCl3/CH3OH/NH4OH (90/10/0.5 to 90/10/1): Yield 2.2 g (49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07320993B1 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-f468d340df2943e98a80abfe913fb672 |
| Source note | uspto-grants-2008_01 |