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N-Methyl-6-nitro-1,3-benzoxazol-2-amine synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

Stage #1: N-methyl-1,3-benzoxazol-2-aminewith nitric acid at 20; for 8 h;
Stage #2: with sodium hydrogencarbonate in water at 0;

Steps:

29.1

2-Methylaminobenzoxazole (2.0 g, Hetzheim, Annemarie; Schlaak, G.; Kerstan, Christa., Pharmazie, (1987), 42, 80) was added in portions to conc. nitric acid (15 ml) at room temperature. Stirring was continued over 8 h. The reaction mixture was poured onto crushed ice/sodium hydrogen carbonate with vigorous stirring. The precipitated title compound (1.76 g) was collected by filtration and dried in vacuo at 40° C. m/z (API+): 194 (MH+).

References:

US6699879,2004,B1 Location in patent:Page/Page column 24-25