反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Sodium (4.6 g) was added by portions at 0° C. to methanol (150 mL). The mixture was stirred at room temperature until dissolution. After cooling at 0° C., thiourea (11.0 g) was added by portions and the mixture was stirred until dissolution. Ethyl butyrylacetate (15.8 g) in methanol (200 mL) was added dropwise at 0° C. over 30 minutes. The mixture was refluxed for 9 h, then concentrated under reduced pressure. The residue was dissolved in water. After acidification with acetic acid until pH=6 and stirring for 1 h, the mixture was filtered. The precipitate was successively washed with water and isopropanol, then dried under reduced pressure to afford 2-mercapto-6-propyl-pyrimidin-4-ol (14.1) as white crystals (mp=220° C.).
WORKUP
后处理
- temperatureAfter cooling at 0° C.
- stirringthe mixture was stirred until dissolution
- temperatureThe mixture was refluxed for 9 h
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in water
- stirringAfter acidification with acetic acid until pH=6 and stirring for 1 h
- filtrationthe mixture was filtered
- washThe precipitate was successively washed with water and isopropanol
- customdried under reduced pressure