反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe temperature of the faintly exothermal reaction
- customis adjusted to at most 35° C.
- stirringThe mixture is then stirred for another hour at 25° C.
- additionpoured onto ice/water
- filtrationthe precipitate is suction-filtered
- washwashed with water
- customrecrystallized from methanol with an addition of charcoal
- customto yield 21.7 g (74% of the