反应详情

温度

80 °C

A mixture of 1-(4-bromophenyl)piperazine hydrochloride (1.0 g, 3.61 mmol), formaldehyde (37% aqueous, 3 mL, 39.71 mmol), AcOH (0.23 mL, 3.97 mmol) and MeOH (30 mL) was heated at 80° C. under nitrogen. After 1.5 hours, the mixture was cooled to 0° C. in an ice bath. Methylene chloride (5 mL) was added followed by a slow addition of sodium borohydride (1.91 g, 50.54 mmol) under nitrogen. The mixture was stirred for 1 hour and then poured into a seperatory funnel containing a saturated solution of NH4Cl (25 mL) and CH2Cl2 (50 mL). The layers were separated and the aqueous layer was extracted with CH2Cl2 (2×50 mL). The extracts were dried (Na2SO4), filtered and concentrated to to give the sub-title compound (900 mg, 97%) which was used without further purification.

1. temperaturethe mixture was cooled to 0° C. in an ice bath
2. additionpoured into a seperatory funnel
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with CH2Cl2 (2×50 mL)
5. dry with materialThe extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated