Lithium hydroxide, monohydrate → HCID 59380363, compound

Participants

Reaction Steps

To a stirring solution of {4-[3-chloro-4-(3-fluoro-benzyloxy)-phenylamino]-benzo[4,5]thieno[2,3-d]pyrimidin-7-yl}-acetic acid ethyl ester (400 mg, 0.766 mmol) in THF (10 mL) was added a solution of lithium hydroxide monohydrate (161 mg, 3.83 mmol) in water (3 mL), and the resulting mixture was stirred at rt overnight. The solvent was evaporated, and aq. NaOH (0.2 N, 5 mL) was added to the residue, and the mixture was washed with diethyl ether (2×8 mL). The pH of the aqueous layer was adjusted to 5 by addition of 0.5 N HCl, and it was then extracted with EtOAc (3×25 mL). The combined organic layers were dried (Na2SO4) and concentrated to give the product as a slightly brown solid. (350 mg, 93%). LCMS RT=3.66 min, [M+H]+=494.1.

Provenance & Evidence