HRID441825

反应详情

EQUATION

反应方程式

HRID 441825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 15.4 g (0.1 mol) of 3-methyl-4-methylmercaptophenol in 30 ml of dimethylformamide, 13.8 g (0.1 mol) of potassium carbonate powder are added, and then a solution of 17.6 g (0.1 mol) of 1-methyl-2-chloromethyl-5-nitro-imidazole in 40 ml of dimethylformamide is added dropwise while stirring at 25° C. The temperature of the faintly exothermal reaction is adjusted to at most 35° C. by cooling with ice water. The mixture is then stirred for another hour at 25° C., poured onto ice/water, the precipitate is suction-filtered, washed with water and recrystallized from methanol with an addition of charcoal to yield 21.7 g (74% of the theoretical yield) of 1-methyl-2-(3-methyl-4-methylthiophenyl-oxymethyl)-5-nitro-imidazole in the form of yellow crystals, m.p. 108° C.

WORKUP

后处理

  1. customThe temperature of the faintly exothermal reaction
  2. customis adjusted to at most 35° C.
  3. stirringThe mixture is then stirred for another hour at 25° C.
  4. additionpoured onto ice/water
  5. filtrationthe precipitate is suction-filtered
  6. washwashed with water
  7. customrecrystallized from methanol with an addition of charcoal
  8. customto yield 21.7 g (74% of the