反应详情

To mixture of 1-(3-bromo-5-fluorophenyl)piperazine (2.91 g, 11 mmol) in MeOH (50 mL) was added (1-ethoxycyclopropoxy)trimethylsilane (13.5 mL, 67.2 mmol), acetic acid (6.5 mL, 112 mmol) and NaBCNH4 (1.0 M in THF) (51 mL, 50.4 mmol). The resulting mixture was heated to 70 C overnight and concentrated in vacuuo to give crude residue which was diluted with EtOAc and washed with 1 N NaOH followed by brine. The organic layer was separated, dried with anhydrous MgSO4, filtered and concentrated in vacuo to give desired 1-(3-bromo-5-fluorophenyl)-4-cyclopropylpiperazine in quantitative yield.

1. temperatureThe resulting mixture was heated to 70 C overnight
2. concentrationconcentrated in vacuuo
3. customto give crude residue which
4. washwashed with 1 N NaOH
5. customThe organic layer was separated
6. dry with materialdried with anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo