Lithium hydroxide, monohydrate → HCID 56961342, compound

Participants

Reaction Steps

Lithium hydroxide monohydrate (0.188 g) was added to a solution of ethyl 2-(2-trifluoromethylbenzenesulphonylamino)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate (Intermediate 27, 0.194 g) in dioxane (1 ml) and water (1 ml) and the mixture was stirred at room temperature for 16 hours. The mixture was then warmed to 60° C. for 1 hour and finally heated in the microwave at 160° C. for 15 minutes. After cooling to room temperature the volatile components were removed under reduced pressure. The residual solution was acidified with aqueous hydrochloric acid (1M) and directly purified by preparative HPLC(C18), eluting with a mixture of methanol and water containing 0.1% formic acid and a gradient of 40-95% to give 2-(2-trifluoromethylbenzenesulphonylamino)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylic acid (0.015 g) as a white solid.

Provenance & Evidence