Hydroxylamine → HCID 10063584, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 7-(4-chloro-benzenesulfinyl)-heptanoic acid ethyl ester (0.5 g, 1.6 mmol) in distilled THF (10 mL) containing 50% aqueous hydroxylamine (0.9 mL, 13.6 mmol) was added at 0° C. a solution of potassium hydroxide in methanol (2.5 mL, 1M, 2.5 mmol) in a dropwise manner. After stirring at 0° C. for 1 h, distilled water (10 mL) was added and the mixture was made neutral by dropwise addition of concentrated hydrochloric acid (10 M) at 0° C. The aqueous solution was extracted with ethyl acetate (2×25 mL) and the combined extracts were washed with brine (25 mL), dried over anhydrous MgSO4, filtered and evaporated to dryness. The residue was recrystallised from ethyl acetate to give the title compound (0.4 g, 83%) as a white powder, mp 103-105° C.

Provenance & Evidence