Aluminium lithium hydride → HCID 178521032, compound

Temperature

0 °C

A solution of the compound prepared in Step 2, above (1.29 g, 5 mmol) in diethyl ether (100 ml) was added dropwise to a stirred suspension of LiAlH4 (0.23 g, 6 mmol) in diethyl ether (20 ml) over 30 minutes at room temperature under a nitrogen atmosphere. The reaction mixture was stirred for 3 hours, cooled to 0° C., and excess hydride was destroyed by addition of water (2.5 ml). To the resultant mixture was added 20% aqueous sulfuric acid (20 ml) and the organic phase was separated. The aqueous phase was extracted with diethyl ether (2×20 ml), and the combined extracts were washed with water (20 ml), saturated aqueous sodium bicarbonate (20 ml) and brine (20 ml), then dried over MgSO4. Evaporation of the solvent gave a clear colorless liquid (quantitative yield) which was used without further purification.

1. customexcess hydride was destroyed by addition of water (2.5 ml)
2. additionTo the resultant mixture was added 20% aqueous sulfuric acid (20 ml)
3. customthe organic phase was separated
4. extractionThe aqueous phase was extracted with diethyl ether (2×20 ml)
5. washthe combined extracts were washed with water (20 ml), saturated aqueous sodium bicarbonate (20 ml) and brine (20 ml)
6. dry with materialdried over MgSO4
7. customEvaporation of the solvent

ORD record

ord-a4f739d7c5a64803bec7b09b33d15bf5

Source dataset

uspto-grants-2001_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06291520B1