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ChemicalBook CAS DataBase List 3-NITROBENZAMIDOXIME

3-NITROBENZAMIDOXIME synthesis

10synthesis methods
-

Yield:5023-94-9 100%

Reaction Conditions:

with hydroxylamine in ethanol;water at 80; for 5 h;

Steps:

4.1.2. General Procedure for the Automated Synthesis of Compounds 6 and 7

General procedure: Nitrile (20.00 mmol), ethanol (30.0 mL) and hydroxylamine (50% in water, 2.0 mL) were addedin a 75 mL double jacket reactor from Chemspeed equipped with condenser. The mixture was shakenat 600 rpm for 5 h at 80 °C, then cooled down to 20 °C. The reaction medium was evaporated underreduced pressure and the solid was finally dried overnight in a heated (40 °C) vacuum oven. 3,4-(Methylenedioxy)benzamidoxime (6): White solid, yield: quant. 1H-NMR (300MHz, DMSO) δ ppm:9.51 (s, 1H), 7.22-7.16 (m, 2H), 6.93-6.88 (m, 1H), 6.03 (s, 2H), 5.72 (s, 2H). 13C-NMR (125.75 MHz,DMSO) δ ppm: 150.98, 148.25, 147.56, 127.87, 119.75, 108.30, 106.17, 101.61.

References:

Stevanovic, Strahinja;Sencanski, Milan;Danel, Mathieu;Menendez, Christophe;Belguedj, Roumaissa;Bouraiou, Abdelmalek;Nikolic, Katarina;Cojean, Sandrine;Loiseau, Philippe M.;Glisic, Sanja;Baltas, Michel;García-Sosa, Alfonso T. [Molecules,2019,vol. 24,# 7,art. no. 1282]

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