HRID49581

反应详情

EQUATION

反应方程式

HRID 49581 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5.0 g of 3-bromo-2-methyl-tetrahydrofuran-2-ol and 5.75 g of formamidine acetate were added to 15 ml of N,N-dimethylformamide. 5 g of diethylamine was slowly added to the reaction mixture, which was then stirred for about 4 hours at 80° C. and was distilled in vacuo for about 1 hour at the same temperature. The resulting oily residue was diluted with 25 ml of acetone. 4.95 g of oxalic acid was added to the reaction mixture, which was then stirred for about 1 hour. The resulting solid was filtered and washed with acetone to give 2.5 g of 2-(5-methyl-1H-imidazol-4-yl)ethanol oxalate (yield: 42%).

WORKUP

后处理

  1. distillationwas distilled in vacuo for about 1 hour at the same temperature
  2. additionThe resulting oily residue was diluted with 25 ml of acetone
  3. addition4.95 g of oxalic acid was added to the reaction mixture, which
  4. stirringwas then stirred for about 1 hour
  5. filtrationThe resulting solid was filtered
  6. washwashed with acetone