Lithium Hydroxide → HCID 59406714, compound

Participants

Reaction Steps

42 g (22 mmol) of methyl 4-[1-(3-ethoxycarbonylaminobenzyl)-6-oxo-1,6-dihydropyridazin-3-yl]benzoate (contaminated with triphenylphosphine oxide) are dissolved in 300 ml of tetrahydrofuran and 30 ml of water, 1.6 g (66 mmol) of lithium hydroxide are added, and the mixture is stirred at room temperature for 15 h. The reaction mixture is evaporated. The residue is dissolved in 400 ml of water and 200 ml of ethyl acetate, the organic phase is separated off, and the aqueous phase is extracted with 2×200 ml of ethyl acetate. The organic phase is discarded, conc. HCl is added to the aqueous phase to pH 4-5. During this operation, a precipitate deposits, which is filtered off with suction, washed with water and dried.

Provenance & Evidence