反応 #1755473

反応方程式

propargyl bromide

tert-butyl-1-piperazine carboxylate

propargyl bromide

potassium carbonate

→

yellow oil

収率 46.0%

4-Prop-2-ynyl-piperazine-1-carboxylic acid tert-butyl ester

収率 46.0%

溶媒

dichloromethane

acetonitile

反応条件

後処理

1. 1
   その他The residue was evaporated to dryness
2. 2
   workup.ADDITIONDichloromethane, 50 mL, and water, 50 mL, were added
3. 3
   抽出The reaction mixture was extracted with CH2Cl2, 4×40 mL
4. 4
   乾燥dried over magnesium sulfate
5. 5
   その他evaporate
6. 6
   その他to provide a brown oil
7. 7
   その他purify with a RT Scientific system

実験手順

To a solution of 10.0 g (54.8 mmol) of tert-butyl-1-piperazine carboxylate in 60 mL acetonitile was added 5.20 mL (60.4 mmol) propargyl bromide and 37.9 g (274 mmol) anhydrous potassium carbonate. Additional propargyl bromide, 1.5 mL, was added after stirring for 36 hours at room temperature. The residue was evaporated to dryness. Dichloromethane, 50 mL, and water, 50 mL, were added. The reaction mixture was extracted with CH2Cl2, 4×40 mL, dried over magnesium sulfate, and evaporate to provide a brown oil. The oil was dissolved in dichloromethane and purify with a RT Scientific system using hexane/ethyl acetate gradient to yield 5.5 g (46%) of yellow oil, which ultimately crystallized upon standing.

出典