反应详情

To piperazine-1-carboxylic acid .tert.-butyl ester (3.543 mmol) in EtOH (13 ml), triethylamine (1.5 ml) and 2-chloro-5-ethyl-pyrimidine (3.540 mmol) are added. The mixture is refluxed with stirring for 6 h. After cooling at room temperature, the reaction mixture is quenched with an ice water and extracted with AcOEt. The organic layer is washed with brine, dried over magnesium sulfate and concentrated to give the product in 41% yield. Rf=0.45 (n-hexane:AcOEt=10:1) 1H NMR(400 MHz, CDCl3) δ 1.19 (t, 3H), 1.49 (s, 9H), 2.47 (q, 2H), 3.49 (dd, 4H), 3.76 (dd, 4H), 8.18 (s, 2H)

1. temperatureThe mixture is refluxed
2. customthe reaction mixture is quenched with an ice water
3. extractionextracted with AcOEt
4. washThe organic layer is washed with brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customto give the product in 41% yield