反应详情

温度

90 °C

A suspension of 2-(4-chloro-3-nitrobenzoyl)benzoic acid (0.31 g 1.00 mmol) and glycine ethyl ester hydrochloride (0.69 g, 5.00 mmol) in a solution of 4M aqueous potassium hydroxide (3.8 mL, 15.0 mmol) was heated to 90° C. for 15 hours. The reaction mixture was cooled to room temperature and it was treated with 2M aqueous hydrochloric acid to adjust the pH to ˜5. It was partitioned with ethyl acetate (50 mL) and the organic layer was washed with brine and dried over anhydrous sodium sulfate. Filtration and concentration of the solvent gave 2-({4-[(carboxymethyl)amino]-3-nitrophenyl}carbonyl)benzoic acid (0.26 g, 76% yield) as a white residue. MS (EI) for C16H12N2O7: 342 (M−).

1. temperatureThe reaction mixture was cooled to room temperature
2. customIt was partitioned with ethyl acetate (50 mL)
3. washthe organic layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationFiltration and concentration of the solvent