Lithium Hydroxide → HCID 9930126, compound

Participants

Reaction Steps

A solution of the ester (1.69 g, 4.21 mmole) of Step F, in dry tetrahydrofuran (20 mL) is treated dropwise under nitrogen with 1N-LiOH (12.6 mL) and the mixture is stirred for 3 hours at room temperature (TLC, 19:1 dichloromethane-methanol or 1:1 hexane-ethyl acetate). The solvent is removed, the residue is treated with water and neutralized (to pH 6.5) with 10% acetic acid. The acid is extracted with ethyl acetate (large volume needed) and the extracts are dried (MgSO4) and evaporated to dryness to yield an off-white solid (1.65 g, quantitative yield, m.p. 190°-193° C., dec.). Recrystallization from ethyl acetate provides a white solid (1.32 g, 80%, m.p. 195°-196° C. dec.). The analytical sample is dried in vacuo at 40° C.

Provenance & Evidence