2086-26-2

30777-85-6

2086-26-2

General procedure for the synthesis of 4-nitrobenzylhydroxylamine hydrochloride from 2-((4-nitrobenzyl)oxy)isoindoline-1,3-dione: Compound 18 (2.00 g, 6.71 mmol) was suspended in EtOH (10 mL), and concentrated aqueous hydrochloric acid (20 mL) was slowly added under magnetic stirring. The reaction mixture was heated to reflux for 3 hours. After completion of the reaction, it was slightly cooled and H2O (30 mL) was added, followed by washing with CHCl3 (20 mL × 1). The aqueous phase was separated and concentrated under reduced pressure to afford 4-nitrobenzylhydroxylamine hydrochloride 19 (1.37 g, quantitative yield) as a milky white solid with melting point 179.1-205.9 °C (literature value 217 °C).1H NMR (300 MHz, DMSO-d6) δ 11.37 (br s, 2H), 8.26 (d, J=8.6 Hz, 2H), 7.68 (d , J=8.6 Hz, 2H), 5.22 (s, 2H).