Hydrochloric Acid → 2-(Propylthio)pyrimidine-4,6-diol

関与物質

反応条件

反応手順

2-Thiobarbituric acid (100 g) was added to water (250 ml) under stirring. A solution of sodium hydroxide pellets or flakes (63.13 g) in water (147.35 ml) was added to the resulting mixture over a period of 15 to 20 minutes at 20-25° C. The resulting mass was stirred for 40 minutes at 20-25° C., followed by the addition of water (200 ml). The reaction temperature was raised to 30-35° C., followed by the addition of methanol (200 ml) and propyl iodide (123.36 g) under stirring at 30-35° C. The resulting reaction mixture was stirred for 30 hours at 30-35° C. The reaction was monitored by thin layer chromatography. After completion of reaction, the pH of the reaction mixture was then adjusted to less than 2.0 by the addition of dilute hydrochloric acid (prepared by mixing of 60 ml of concentrated hydrochloric acid with 140 ml of water). The resulting slurry was stirred for 15 hours and the product was isolated by filtration and washed successively with water (4×200 ml). The wet cake was slurried in cyclohexane (500 ml) at boiling temperature for 30 minutes, followed by cooling to 25-30° C. The product was isolated by filtration and washed with cyclohexane (200 ml). The wet product was dried under reduced pressure at 40-45° C. to produce 80 g of 2-propylthio-pyrimidine-4,6-diol as a white powder (Yield: 61.9%).

情報源と証拠