Aluminium lithium hydride → HCID 22607782, compound

Participants

Reaction Steps

To a solution of Example 405A (3.2 g, 8.5 mmol) in THF (20 mL) and ether (30 mL) was slowly added LiAlH4 powder (323 mg, 8.5 mmol) in several portion at rt. While LAH was added a lot of solid material precipitated from the solution and the temperature arises to about 40° C. Water (2 mL) and diluted HCl was added slowly and the mixture was neutralized with NaHCO3 and extracted with ethyl acetate. The organic phase was washed with water and concentrated. The residue was separated by flash chromatography (20-80% EtOAc in hexane) to give the desired product (1.24 g, 42%). MS (DCI) m/z 347, 349 (M+1)+.

Provenance & Evidence