反应详情

温度

0 °C

Tert-Butyl piperazine-1-carboxylate (4.00 g, 21.4 mmol) is dissolved in dichloromethane (40 mL), cooled to 0° C. and treated with acetic anhydride (2.23 mL, 23.6 mmol) over a period of 2 min. The reaction mixture is stirred at 0° C. for 30 min, LCMS analysis used to indicate completion of the reaction and the volatiles evacuated in vacuo. The residue is treated carefully with NaHCO3 (sat. aq., 50 mL), stirred vigorously for 30 min and the resulting mixture extracted with diethyl ether (4×20 mL). The combined organic extracts are dried (MgSO4), filtered and concentrated in vacuo to afford tert-Butyl-4-acetylpiperazine-1-carboxylate as a white solid (4.53 g, 93%). 1H NMR (400 MHz, DMSO-D6) δ ppm 1.39 (s, 9H), 1.99 (s, 3H), 3.22-3.29 (m, 2H), 3.30-3.34 (m, 2H), 3.36-3.41 (m, 4H); ESI-MS: m/z 229.3 (M+H)+.

1. customcompletion of the reaction
2. customthe volatiles evacuated in vacuo
3. additionThe residue is treated carefully with NaHCO3 (sat. aq., 50 mL)
4. stirringstirred vigorously for 30 min
5. extractionthe resulting mixture extracted with diethyl ether (4×20 mL)
6. dry with materialThe combined organic extracts are dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo