HRID733163

反应详情

EQUATION

反应方程式

HRID 733163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling at 0° C.
  2. stirringthe mixture was stirred until dissolution
  3. temperatureThe mixture was refluxed for 9 h
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe residue was dissolved in water
  6. stirringAfter acidification with acetic acid until pH=6 and stirring for 1 h
  7. filtrationthe mixture was filtered
  8. washThe precipitate was successively washed with water and isopropanol
  9. customdried under reduced pressure