HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisobutylaluminum hydride → HCID 46240282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | HCID 11988837 | HCID 11988837 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 46240282 | HCID 46240282 | 11.5% |
Reaction Steps
(6aR,9aS)-5,6a,7,8,9,9a-hexahydro-5-methyl-3-(phenylamino)-2-((4-Pyridin-2-yl)-benzyl)-cyclopent[4,5]imidazo[1,2-a]pyrazolo[4,3-e]pyrimidin-4(2H)-one (26.9 mg, 0.055 mmol) is dissolved in 1 mL of anhydrous THF, and then 400 uL of 1.5 M DIBAL-H in toluene is added dropwise. After the reaction mixture is stirred at room temperature overnight, additional 800 uL of 1.5 M DIBAL-His added to the solution. The reaction mixture is stirred at room temperature for 24 hours, and then quenched with NH4Cl aqueous solution. After routine workup, the mixture is purified by a semi-preparative HPLC to give 3.0 mg of pure product as while solids. MS (ESI) m/z 476.3 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08633180B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-55f1ca06fb774a408d166a0b98eec450 |
| Source note | uspto-grants-2014_01 |