HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → HCID 68671644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68671138 | HCID 68671138 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68671644 | HCID 68671644 | 46.2% |
Reaction Steps
To a solution of {4-[3-(1-Methyl-1H-benzoimidazol-2-yl)-phenyl]-piperazin-1-yl}-(4-methyl-morpholin-3-yl)-methanone (0.06 g, 0.16 mmol) in dry THF (2 mL) at room temperature under a nitrogen atmosphere was added lithium aluminium hydride (LiAlH4) (0.02 g, 0.47 mmol). The reaction was heated at reflux for 2 h and other LiAlH4 (0.01 g, 0.24 mmol). After 30 min the solution was cooled to room temperature, quenched with 10% NaOH (3 mL) and then extracted with dichloromethane (3×3 mL) The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude was then purified by Preparative HPLC to obtain 0.03 g (41%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592463B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-0285b308ca144c02b7ddeba324a65153 |
| Source note | uspto-grants-2013_11 |