反应详情

温度

60 °C

1-(2,3-Dihydro-1,4-benzodioxin-2-ylmethyl)piperazine (4.7 g, 20 mmole) and 2,6-dichloropyrazine (3.0 g, 20 mmole) were combined in 200 ml of dimethylformamide and 2.6 g (20 mmole) of diisopropylethylamine was added. The mixture was heated under nitrogen at 60° C. for 24 hours. The solvent was then removed in vacuum and the residue filtered through 75 g of silica gel with chloroform as the eluent. The product-containing fractions were concentrated in vacuum and the residue was crystallized from methanol with addition of 4N isopropanolic HCl and recrystallized from methanol to give 4.26 g of the title compound as the monohydrochloride, m.p. 270°-280° C.

1. customThe solvent was then removed in vacuum
2. filtrationthe residue filtered through 75 g of silica gel with chloroform as the eluent
3. concentrationThe product-containing fractions were concentrated in vacuum
4. customthe residue was crystallized from methanol with addition of 4N isopropanolic HCl
5. customrecrystallized from methanol