反应详情

温度

-78 °C

2-(4-(1,2,3,4-Tetrahydro-8-methoxy-2-naphthalenyl)-1-piperazinyl]-pyrimidine hydrochloride (1.62 g, 5.0 mmole) was dissolved in 185 ml of methylene chloride and cooled to -78° C. in a dry ice/acetone bath. A mixture of 15 ml of 1 M boron triboromide and 15 ml of methylene chloride was added. The reaction mixture was allowed to come to room temperature and it was then stirred for three days. The reaction was then poured into a saturated NaHCO3 solution and the product extracted with 600 ml of chloroform. This solution was dried over MgSO4, filtered, and concentrated in vacuum. The residue was column chromatographed on 100 g of silica gel with 5% methanol/chloroform and the crude title compound thus obtained was crystallized from isopropanol with addition of 4 N isopropanolic HCl and recrystallized from acetone to give 1.1 g of the title compound as the hydrochloride, monohydrate, m.p.>300° C.

1. additionwas added
2. customto come to room temperature
3. extractionthe product extracted with 600 ml of chloroform
4. dry with materialThis solution was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuum
7. customchromatographed on 100 g of silica gel with 5% methanol/chloroform
8. customthe crude title compound thus obtained
9. customwas crystallized from isopropanol with addition of 4 N isopropanolic HCl
10. customrecrystallized from acetone