反応 #332183

反応方程式

4-iodoaniline

piperazine-1-carboxylic acid tert-butyl ester

potassium phosphate

ethylene glycol

→

43a

収率 43.3%

4-(4-aminophenyl)-piperazine-1-carboxylic acid tert-butyl ester

収率 43.3%

溶媒

2-propanol

反応条件

後処理

1. 1
   その他was placed under argon in a sealed-tube
2. 2
   温度After being cooled to room temperature
3. 3
   洗浄the medium was washed with water (50 ml)
4. 4
   抽出extracted with ethyl acetate (100 ml)
5. 5
   乾燥The organic layer was dried over MgSO4
6. 6
   濃縮concentrated
7. 7
   その他chromatographed (dichloromethane:acetone, 70:30)

実験手順

A mixture of 4-iodoaniline (0.654 g, 3 mmol), piperazine-1-carboxylic acid tert-butyl ester (0.67 g, 3.6 mmol), potassium phosphate (1.272 g, 6 mmol), ethylene glycol (0.33 ml) and copper iodide (0.03 g, 0.15 mmol) in 2-propanol (3 ml) was placed under argon in a sealed-tube and heated to 80° C. for 30 hours. After being cooled to room temperature, the medium was washed with water (50 ml) and extracted with ethyl acetate (100 ml). The organic layer was dried over MgSO4, concentrated and chromatographed (dichloromethane:acetone, 70:30) to yield 43a (0.36 g, 1.3 mmol, 43%) as a yellow powder.

出典