反応 #5825

反応方程式

dimethylformamide

homopiperazine

sodium bicarbonate

benzyloxycarbonyl chloride

→

title compound

収率 65.5%

N-Benzyloxycarbonylhomopiperazine

収率 65.5%

溶媒

water

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at a room temperature overnight
2. 2
   その他After evaporating off dimethylformamide under a reduced pressure
3. 3
   抽出the reaction mixture was extracted three times with 100 ml of chloroform
4. 4
   乾燥the extract was dried over magnesium sulfate
5. 5
   その他evaporated
6. 6
   その他to remove the solvent under a reduced pressure
7. 7
   洗浄eluted with chloroform/methanol (9:1)

実験手順

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.

出典