反应详情

Thiourea (80 g, 1.05 mol) and dimethyl acetylsuccinate (188 g, 1.0 mol) are added at room temperature to a solution of sodium (46 g, 2.0 mol) in methanol (800 ml). The reaction mixture is refluxed for 14 hours. The crystalline precipitate is filtered and added with stirring to a concentrated aqueous solution of hydrochloric acid (250 ml). The resulting colorless crystalline precipitate is filtered, washed with methanol and dried at high vacuum to give 4-hydroxy-2-mercapto-6-methyl-5-pyrimidinyl acetic acid (190 g, 95%). 1H-NMR (DMSO):12.4 (s, 1H); 12.3 (s, 1H); 3.4 (s, 2H); 2.1 (s, 3H).

1. temperatureThe reaction mixture is refluxed for 14 hours
2. filtrationThe crystalline precipitate is filtered
3. additionadded
4. filtrationThe resulting colorless crystalline precipitate is filtered
5. washwashed with methanol
6. customdried at high vacuum