HRID1813886

反应详情

EQUATION

反应方程式

HRID 1813886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 mmol of piperazine was dissolved in 10 ml of DMF and 1.05 mmol of 1,3 di-p-tolylcarbodiimide was added. After 0.5 h. of stirring at room temperature, a small precipitation was filtered off and washed twice with 1 ml of DMF. The filtrates were collected and kept at room temperature overnight. To the DMF solution, 50 ml of water was added. The precipitated solid was filtered and washed with water. The solid was dissolved in ethyl acetate (20 ml) and 0.2 ml of conc. HCl conc. was added. The product began to precipitate within 15 min. After 1 hour, the precipitate was filtered and washed with ethyl ether. Yield=76%.

WORKUP

后处理

  1. customa small precipitation
  2. filtrationwas filtered off
  3. washwashed twice with 1 ml of DMF
  4. customThe filtrates were collected
  5. waitkept at room temperature overnight
  6. additionTo the DMF solution, 50 ml of water was added
  7. filtrationThe precipitated solid was filtered
  8. washwashed with water
  9. dissolutionThe solid was dissolved in ethyl acetate (20 ml)
  10. addition0.2 ml of conc. HCl conc. was added
  11. customto precipitate within 15 min
  12. waitAfter 1 hour
  13. filtrationthe precipitate was filtered
  14. washwashed with ethyl ether