反应详情

A solution of tert-butyl piperazine-1-carboxylate (334, 1 g, 5.37 mmol), 3-(bromomethyl)benzonitrile (335, 1.26 g, 6.45 mmol) and K2CO3 (1.48 g, 10.74 mmol) in EtOH (20 mU was refluxed for four hours. The reaction mixture was then concentrated, diluted with EtOAc (20 ml.) and washed with water (20 mL). The organic phase was separated, dried with Na2SO4, filtered and concentrated. Crude product was purified by flash chromatography using the gradient 10%-25% EtOAc in hexanes as an eluent to afford the title compound 336 (1.374 g 85%). MS: calc: 301.3; found: 302.1 (M+H)

1. concentrationThe reaction mixture was then concentrated
2. additiondiluted with EtOAc (20 ml.)
3. washwashed with water (20 mL)
4. customThe organic phase was separated
5. dry with materialdried with Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customCrude product was purified by flash chromatography