Sulfuric Acid → HCID 24178416, compound

Participants

Reaction Steps

2.063 g (R)-5-[2-(5,6-diethyl-indan-2-ylamino)-1-hydroxyethyl]-8-hydroxy-1H-quinolin-2-one base (5.256 mmoles) are dissolved in 12 ml acetic acid at 50° C. A solution of 0.526 g sulfuric acid 98% (5.256 mmoles) in 4 ml acetic acid is adder dropwise, at constant flow rate, over 5 minutes. The clear solution is allowed to cool. Crystallization takes spontaneously place at ca. 35° C. The suspension is stirred for 18 h at room temperature and then filtered. The crystals are washed with 4 ml acetic acid and 10 ml ethylacetate. The salt is dried first for 20 hours at 70° C. and ca. 10 mbar and then for 2 hours at 60° C. and ca. 1 mbar. Yield: 2.31 g white powder (86.9%)

Provenance & Evidence