HRID1663460

反应详情

EQUATION

反应方程式

HRID 1663460 的结构方程式

PROCEDURE

实验过程

Part A: A mixture of sodium metal (1.55 g, 67.4 mmol) and EtOH (15.0 mL, 257 mmol) was stirred at RT until nearly all sodium had reacted. Diethyl fluoromalonate (3.54 mL, 22.4 mmol) was added followed by acetamidine hydrochloride (2.14 g, 22.7 mmol). The reaction mixture was heated at reflux for 3 h, cooled to RT and concentrated under reduced pressure. The residue was diluted with water (ca. 50 mL) and acidified (pH=2) with 6M aqueous HCl, and the mixture was stirred at RT for 1 h as a precipitate formed. The solids were collected by suction filtration and washed with water. Excess solvent was removed in vacuo to give 4,6-dihydroxy-5-fluoro-2-methylpyrimidine (2.08 g, 64%) as a light gray solid. LCMS (m/z): 145 (M+H)+

WORKUP

后处理

  1. customhad reacted
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux for 3 h
  4. concentrationconcentrated under reduced pressure
  5. additionThe residue was diluted with water (ca. 50 mL)
  6. customformed
  7. filtrationThe solids were collected by suction filtration
  8. washwashed with water
  9. customExcess solvent was removed in vacuo