Citric Acid → HCID 136481381, compound

Participants

Reaction Steps

A stirred mixture of the title compound of Example 5A (15.0 g, 26.5 mmol) and acetone (150 ml) was heated under reflux, then filtered. To the stirred filtrate was added a filtered solution of citric acid (5.10 g, 26.5 mmol) in a mixture of acetone (75 ml) and water (7.5 ml), then the reaction mixture heated under reflux for 75 minute and allowed to cool. The resulting suspension was granulated for 1 hour and filtered, then the solid thus obtained washed with acetone (20 ml) and dried at 45° C. to provide the title compound (18.33 g, 91%) as a white solid, m.p. 185° C. Found: C, 53.84; H, 5.71; N, 12.89. C28H35N7O4S; C6H8O7 requires C, 53.89; H, 5.72; N, 12.94. δ(DMSOd6): 0.95 (6H, m), 1.20 (3H, t), 1.72 (2H, m), 2.40-2.73 (10H, m), 2.96 (4H, m), 4.11 (2H, t), 5.68 (2H, s), 7.21 (1H, d), 7.34 (2H, m), 7.82(3H, m), 8.51 (1H, d), 11.72 (1H, s).

Provenance & Evidence