HRID370283

反应详情

EQUATION

反应方程式

HRID 370283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

15.13 g of (2-chloroethoxy)acetamide (0.11 mol), 14.6 ml of ethyl piperazine carboxylate (0.1 mol), 23.3 g of sodium carbonate (0.22 mol) and 1.0 g of potassium iodide in 25 ml of toluene are introduced into a round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. The mixture is heated at the reflux temperature for 4 hours and is allowed to cool to room temperature. The reaction is continued, still with stirring, for a further 16 hours. 100 ml of isopropanol are added and the solid materials formed are filtered off. The solvent is evaporated from the filtrate under reduced pressure to dryness. The product obtained after evaporation of the solvents is recrystallized from toluene. 21.35 g of ethyl 4-(2-carbamoylmethoxyethyl)piperazine-1-carboxylate are obtained.

WORKUP

后处理

  1. temperaturecooled condenser and a mechanical stirrer
  2. temperatureThe mixture is heated at the reflux temperature for 4 hours
  3. customthe solid materials formed
  4. filtrationare filtered off
  5. customThe solvent is evaporated from the filtrate under reduced pressure to dryness
  6. customThe product obtained
  7. customafter evaporation of the solvents
  8. customis recrystallized from toluene