Lithium hydroxide, monohydrate → HCID 71227271, compound

Participants

Reaction Steps

To a solution of [4-(3-chloro-4-methoxy-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester (0.76 g, 2.24 mmol in 6 mL of THF and 2 mL of methanol) was added LiOH.H2O (0.47 g, 11.2 mmol in 3 mL of water) and the reaction mixture was stirred at ambient temperature for 1.5 hours. The solvent was removed in vacuo then diluted with 20 mL of water (pH 14). The residue was treated with 12 mL of 1 N HCl (pH 4), frozen at −78° C. and lyophilized for 24 hours to yield the title compound (0.70 g, 2.1 mmol). MS (ESI) m/z 312.4 (M+H+); HPLC (Novapak 150×3.9 mm C-18 column: mobile phase: 35-90% acetonitrile/water with 0.1% TFA, at 2 mL/min over 2 min.) t 1.81 min.

Provenance & Evidence