HRID1090323

反应详情

EQUATION

反应方程式

HRID 1090323 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a chilled (0°-5° C.) solution of 3.3 g (0.014 mol) of 2-[[(phenyl)methyl]thio]-1H-imidazo[4,5-c]pyridine in 50 mL of chloroform and 5 mL of methanol was added dropwise a solution containing 2.78 g (0.014 mol) of m- chloroperoxybenzoic acid in 50 mL of chloroform. The reaction mixture was then stirred at room temperture for 45 minutes. Approximately one half of the chloroform was removed in a rotary evaporator and the reaction mixture was then poured into 200 mL of ether. The reaction mixture was cooled in ice. The precipitate that formed was collected and amounted to 1.78 g. The product was suspended in aqueous 10% sodium bicarbonate solution, filtered and was air dried overnight. The product amounted to 1.39 g. An analytical sample (m.p. 190°-193° C.) was obtained by recrystallization from ethanol.

WORKUP

后处理

  1. additionwas added dropwise a solution
  2. customApproximately one half of the chloroform was removed in a rotary evaporator
  3. additionthe reaction mixture was then poured into 200 mL of ether
  4. temperatureThe reaction mixture was cooled in ice
  5. customThe precipitate that formed
  6. customwas collected
  7. filtrationfiltered
  8. customdried overnight
  9. customAn analytical sample (m.p. 190°-193° C.) was obtained by recrystallization from ethanol