HRID1707623

反应详情

EQUATION

反应方程式

HRID 1707623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 1-piperazinecarboxylate (77.3 g, 0.28 mole), 1-decanol methanesulfonate (77.3 g, 0.28 mole) from the condensation of 1-decanol with methane sulfonyl chloride, K2CO3 (39.0 g, 0.28 mole), and 500 mL of EtOH were combined and refluxed for 2 days under N2. After cooling to room temperature, the reaction was partitioned between water and Et2O. The organic layer was separated, washed 3 times with water, dried over Na2SO4 and stripped of all solvent under reduced pressure to yield the crude product oil. Chromatographic purification of the crude oil gave 53.4 g of ethyl 4-decyl-1-piperazinecarboxylate.

WORKUP

后处理

  1. temperaturerefluxed for 2 days under N2
  2. customthe reaction was partitioned between water and Et2O
  3. customThe organic layer was separated
  4. washwashed 3 times with water
  5. dry with materialdried over Na2SO4
  6. customto yield the crude product oil
  7. customChromatographic purification of the crude oil