HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 11547510, compound → HCID 11532855, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 11547510 | HCID 11547510 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11532855 | HCID 11532855 | — |
Reaction Steps
To a solution of 20 (0.2 g, 0.416 mmol, 1.0 eq) in tetrahydrofuran (10 mL) under nitrogen atmosphere at 0° C. was added lithium aluminum hydride (1.0 M in THF, 1.6 mL, 1.60 mmol, 4.0 eq). The mixture was slowly warmed up to room temperature over 2.5 hours, and LC/MS showed the reaction was complete. The reaction was quenched with ice chips, and then water/ethyl acetate was added. The aqueous layer was extracted with ethyl acetate (2×20 mL), and the combined organic layer was washed with water (20 mL), brine (20 mL) and dried over anhydrous MgSO4. The solvent was removed under reduced pressure, and the residue was purified by column chromatography (neutral aluminum gel, 2% methanol in dichloromethane).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07671052B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-1cf87582fd524c2683585ce0027cd8c6 |
| Source note | uspto-grants-2010_03 |