HRID5729

反应详情

EQUATION

反应方程式

HRID 5729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.

WORKUP

后处理

  1. stirringthe mixture was stirred at a room temperature overnight
  2. customAfter evaporating off dimethylformamide under a reduced pressure
  3. extractionthe reaction mixture was extracted three times with 100 ml of chloroform
  4. dry with materialthe extract was dried over magnesium sulfate
  5. customevaporated
  6. customto remove the solvent under a reduced pressure
  7. washeluted with chloroform/methanol (9:1)