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ChemicalBook CAS DataBase List NSC 11344
5416-12-6

NSC 11344 synthesis

2synthesis methods
-

Yield:5416-12-6 94%

Reaction Conditions:

with sulfuric acid;nitric acid;acetic acid at 0 - 20; for 1 h;

Steps:

10 N-(2,6-dimethyl-3-nitro-phenyl)acetamide

N-(2,6-dimethylphenyl)acetamide (10 g, 60 mmol, 1.0 eq) was dissolved in a mixture of H2S04 (40 mL) and acetic acid (20 mL) at 0°C. A mixture of HN03 (10 mL) and H2S04 (8 mL) was added drop wise with stirring. The reaction was allowed to warm to room temperature and stirred for a further lh. The reaction was quenched by pouring into ice water, and the solid that formed collected by filtration to give the title compound as a yellow solid (12 g, 94 %).LC-MS: 209.1 [M+H]1H MR (400 MHz, DMSO-d6) ? 9.58 (s, 1H), 7.75 (d, J = 8.4 Hz, 1H), 7.33 (d, J = 8.4 Hz, 1H), 2.23 (s, 3H), 2.23 (s, 3H), 2.09 (s, 3H)

References:

WO2013/37705,2013,A2 Location in patent:Page/Page column 80; 81