HRID1090322

反应详情

EQUATION

反应方程式

HRID 1090322 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.26 g (0.055 g atom) of sodium in 300 mL of methanol was added 7.56 g (0.05 mol) of 2-mercapto-1H-imidazo[4,5-c]pyridine with stirring. After 20 minutes, the reaction mixture was evaporated to dryness in a rotary evaporator. Dimethyl formamide (200 mL) was added to the residue. To the resulting solution was added dropwise 6.33 g (0.05 mol) of benzylchloride. The reaction mixture was stirred for 5 hours at room temperature and was then poured into 1500 mL of water. The product was removed by filtration and amounted to 9.5 g, m.p. 175°-177° C. The product was triturated with hot ethyl acetate and refiltered. The product amounted to 8.11 g, m.p. 175°-177° C. A portion recrystallized from ethyl acetate gave the analytical sample (m.p. 175°-177° C.).

WORKUP

后处理

  1. customthe reaction mixture was evaporated to dryness in a rotary evaporator
  2. additionDimethyl formamide (200 mL) was added to the residue
  3. stirringThe reaction mixture was stirred for 5 hours at room temperature
  4. customThe product was removed by filtration
  5. customThe product was triturated with hot ethyl acetate
  6. customA portion recrystallized from ethyl acetate
  7. customgave the analytical sample (m.p. 175°-177° C.)