反应详情

To a solution of 1,1-dimethylethyl 1-piperazinecarboxylate (72.8 g, 390 mmol) in acetonitrile (1.4 L) was added methyl vinyl sulfone (50 g, 470 mmol) and Na2CO3 (124 g, 1170 mmol) and the mixture was refluxed overnight. Then the mixture was cooled to rt, and poured into H2O and extracted with EtOAc. The organic layer was dried over Na2SO4 and the solvent was removed under reduced pressure to give the title compound (106 g, 93% yield). 1H NMR (400 MHz, CDCl3) δ ppm 1.41-1.57 (m, 9H), 2.39-2.51 (m, 4H), 2.88 (t, J=8.4 Hz, 2H), 3.02 (s, 3H), 3.14 (t, J=8.4 Hz, 2H), 3.35-3.50 (m, 4H).

1. temperaturethe mixture was refluxed overnight
2. extractionextracted with EtOAc
3. dry with materialThe organic layer was dried over Na2SO4
4. customthe solvent was removed under reduced pressure