反应详情

温度

70 °C

N-Ethyl-N-phenyl-5-ethyl-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-3-quinolinecarboxamide (5.0 g, 14.2 mmol) was dissolved in a mixture of 1M NaOH (14.26 mmol, 14.26 ml) and ethanol (30 ml), and pH was adjusted to 7.5. The solution was heated to 70° C. and calcium acetate hydrate (1.05 eq., 7.5 mmol, 1.335 g) in water (7 ml) was added dropwise during 5 min. The heating was discontinued and the mixture was stirred at room temperature for 1 h, the crystals were filtered, washed with ethanol/water 1/1, and dried under vacuum to afford the title compound (5.16 g, 98% yield). Anal. Calcd for C42H42N4O6Ca: C, 68.3; H, 5.73; N, 7.58. Found C, 68.4; H, 5.72; N, 7.63. EDTA-titriometric determination of calcium gave a content of 5.42% (theoretical content is 5.42%).

1. filtrationthe crystals were filtered
2. washwashed with ethanol/water 1/1
3. customdried under vacuum