Aluminium lithium hydride → HCID 59160998, compound

Participants

Reaction Steps

1.90 g (3.75 mmol, 87% pure) of the compound from Example 3A are dissolved in 15 ml of diethyl ether and added dropwise to a suspension of 170.9 mg (4.50 mmol) of lithium aluminum hydride in 15 ml of diethyl ether. The mixture is then stirred at RT for 20 h. A further 136.7 mg (3.60 mmol) of lithium aluminum hydride are then added, and the mixture is stirred at RT for another 20 h. The mixture is then triturated with 257 μl of water and 257 μl of 15% strength aqueous potassium hydroxide solution. A further 10 ml of water are added, and the phases are separated. The organic phase is dried over magnesium sulfate. The solvent is removed on a rotary evaporator and the residue is purified chromatographically on silica gel 60 (mobile phase: gradient cyclohexane/ethyl acetate 50:1→10:1).

Provenance & Evidence