HRID1972390

反应详情

EQUATION

反应方程式

HRID 1972390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 250 mL round-bottomed flask was charged with methyl N-(tert-butoxycarbonyl)-3-(tetrahydro-2H-pyran-4-yl)-alanylglycinate (3.00 g, 8.71 mmol), 10 mL of CH2Cl2, and 5 mL of TFA. After 10 min, the mixture was concentrated then re-dissolved in MeOH (50 mL) and triethylamine (10 mL) and then heated at reflux for 18 h. After that time, the white precipitate formed was collected by filtration to give 3-(tetrahydro-2H-pyran-4-ylmethyl)-2,5-piperazinedione (1.44 g) as a white solid.

WORKUP

后处理

  1. concentrationthe mixture was concentrated
  2. dissolutionthen re-dissolved in MeOH (50 mL)
  3. temperaturetriethylamine (10 mL) and then heated
  4. temperatureat reflux for 18 h
  5. customAfter that time, the white precipitate formed
  6. filtrationwas collected by filtration