* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference:
[1] Bulletin des Societes Chimiques Belges, 1957, vol. 66, p. 276,289
2
[ 17758-52-0 ]
[ 4595-61-3 ]
Reference:
[1] Bulletin des Societes Chimiques Belges, 1957, vol. 66, p. 276,289
3
[ 17758-52-0 ]
[ 2036-41-1 ]
Reference:
[1] Bulletin des Societes Chimiques Belges, 1957, vol. 66, p. 276,289
4
[ 636-26-0 ]
[ 17758-52-0 ]
Yield
Reaction Conditions
Operation in experiment
97%
With ammonia In water for 16 h; Reflux
To a suspension of 4-hydroxy-2-mercapto-5-methylpyrimidine (1.0 g, 7.0 mmol) in water (50 mL) and ammonia (3 mL) was added a suspension of Raney Nickel in water (20 mL). The mixture was heated at reflux for 16 h, then hot filtered through celite (10 g) and washed with water (3 * 25 ml_). The filtrate was evaporated and the resultant solid was azeotroped with toluene (2 x 50 ml.) to furnish a white solid (0.75 g, 97percent).
With ammonia;Raney-Nickel; In water; for 16.0h;Reflux;
To a suspension of 4-hydroxy-2-mercapto-5-methylpyrimidine (1.0 g, 7.0 mmol) in water (50 mL) and ammonia (3 mL) was added a suspension of Raney Nickel in water (20 mL). The mixture was heated at reflux for 16 h, then hot filtered through celite (10 g) and washed with water (3 * 25 ml_). The filtrate was evaporated and the resultant solid was azeotroped with toluene (2 x 50 ml.) to furnish a white solid (0.75 g, 97%).
A mixture of 5-methyl-3/-/-pyrimidin-4-one (0.60 g, 3.6 mmol) and phosphorous oxychloride (2.0 ml.) was heated at 90 0C for 2.5 h. The mixture was evaporated to dryness under reduced pressure and the resultant solid was purified by sublimation under reduced pressure to furnish the title compound as a white solid. This compound was unstable to air and was used immediately in the next step.