Water → HCID 13432890, compound

Participants

Reaction Conditions

Reaction Steps

Under cold conditions (ice bath) and under an inert atmosphere, 60 ml (61.6 mmol) of a solution of lithium aluminium hydride (1N) in THF are added dropwise to 11 g (30.8 mmol) of the compound obtained from step 1.8 suspended in THF (60 ml). After addition, the reaction mixture is heated for 3 hours at 70° C. and then cooled to 0° C. 2.8 ml of water (formation of a precipitate), 2.8 ml of NaOH solution (1N) and 8.3 ml of water are then successively added dropwise. This mixture is stirred for 30 minutes and then filtered, the solid is rinsed with THF (10 ml) and the filtrate is then concentrated under reduced pressure. 10 g of compound are obtained in the form of a bright yellow powder, which is used without further purification in the following step. Yield=95%. Melting point: 100° C.

Provenance & Evidence