Hydrochloric Acid → HCID 15480017, compound

Participants

Reaction Conditions

Reaction Steps

0.2 M Aqueous potassium hydroxide solution (5 mL, oxygen was removed by addition of 15 mg of sodium hydrosulfite in advance) was mixed with 2-(3-carboxymethyl-4-iodophenyl)propionic acid (prepared in Example 12, 40.7 mg, 0.122 mmol.) and thiosalicylic acid (37.3 mg, 0.242 mmol.). The resulting mixture was heated for 20 hours under reflux (temperature: approx. 100° C.) after addition of 10 mg of powdery copper. The reaction mixture was cooled, made acidic by addition of hydrochloric acid, and extracted with ethyl acetate. The ethyl acetate portion was washed with an aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated to leave a residue. The residue was subjected to silica gel column chromatography (Wako Gel C-200, Wako Jyunyaku Industry Co., Ltd., hexane/ethyl acetate/acetic acid=7/3/1, v/v/v) to obtain 40.6 mg (0.084 mmol., yield: 69%) of the desired compound.

Provenance & Evidence