反应详情

Formaldehyde (1.84 ml in solution) is added to a solution of 1-(2-methoxyphenyl)-piperazine (4.77 g, 24.3 mmol) in 1,2-dichloroethane. NaHB(OAc)3 (7.59 g, 34 mmol) is then added portionwise. After stirring at RT overnight, the reaction is quenched by addition of a saturated solution of NaHCO3. The mixture is extracted several times with EtOAc and the combined organic layers are washed with brine, dried over Na2SO4, filtered and the filtrate is concentrated in vacuo to afford the title compound as a colorless oil, Rt=0.615 min (Acquity HPLC BEH C18, 2.1×50 mm, 1.7 micron, detection 215 nM, 0.1 min 2% CH3CN in H2O, 2% to 100% CH3CN in H2O in 1.5 min, 0.4 min 100% CH3CN+0.1% TFA, flow rate 1.0 ml/min); MS: 207 (M+1)+.

1. customthe reaction is quenched by addition of a saturated solution of NaHCO3
2. extractionThe mixture is extracted several times with EtOAc
3. washthe combined organic layers are washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationthe filtrate is concentrated in vacuo