Nitric Acid → HCID 131729650, compound

Participants

Reaction Conditions

Reaction Steps

Concentrated sulfuric acid (240 mL, 4.2 mol) was added to a solution of compound of Example 1i (37 g, 0.105 mol) in concentrated nitric acid (1100 mL, 17.34 mol) at 5° C. The reaction mixture was stirred at 5° C. for 25 min, and then at 40° C. for 4.5 h. Reaction mixture was quenched into ice water (2500 mL), the solid precipitated was filtered, washed with water till filtrate was neutral to pH and dried to obtain the title compound. Yield: 38 g (90.91%); 1H NMR (CDCl3, 300 MHz): δ 2.7 (s, 3H, CH3), 3.90 (s, 3H, OCH3), 4.79 (s, 2H, CH2), 8.10 (s, 1H, Ar), 8.22 (s, 1H, Ar), 8.38 (s, 1H, Ar), 8.48 (s, 1H, Ar); MS: m/e (ES−) 396 (M−1).

Provenance & Evidence