反应详情

温度

0 °C

To a stirred suspension of sodium methoxide (3.48 g) in methanol (40 mL), cooled to 0° C., was added thiourea (3.56 g). The mixture was stirred until it dissolved, then 6-benzyloxy-3-oxo-hexanoic acid ethyl ester (8.52 g in 20 mL methanol) was added slowly. The solution was heated at reflux overnight, cooled to room temperature, and concentrated under vacuum. The residue was dissolved in water (50 mL), acidified to pH 6 with acetic acid, and stirred for 1 h. The precipitate was filtered, washed successively with water (2×20 mL) and isopropanol (2×20 mL), then dried to afford 6-(3-benzyloxy-propyl)-2-mercapto-pyrimidin-4-ol as a white powder (7.94 g). MS m/z 277.1 (M+1), 100%.

1. dissolutiondissolved
2. temperatureThe solution was heated
3. temperatureat reflux overnight
4. temperaturecooled to room temperature
5. concentrationconcentrated under vacuum
6. dissolutionThe residue was dissolved in water (50 mL)
7. stirringstirred for 1 h
8. filtrationThe precipitate was filtered
9. washwashed successively with water (2×20 mL) and isopropanol (2×20 mL)
10. customdried