反应详情

A solution of 2-chloro-4-((tetrahydro-2H-pyran-2-yloxy)methyl)pyridine (8.7 g, 38.2 mmol) and piperazine (16.4 g, 191 mmol) in DIEA (30 mL) was heated at 150° C. for 48 h. The reaction mixture was diluted with H2O (1000 mL), and the solution was extracted with DCM/MeOH (10/1, 3×400 mL). The combined organic layers were washed with H2O (100 mL), and brine (100 mL), dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel column chromatography (DCM:MeOH=15:1) to afford 1-(4-((tetrahydro-2H-pyran-2-yloxy)methyl)pyridin-2-yl) piperazine as yellow oil (8.5 g, 80%). MS (ES+) C15H23N3O2 requires: 277, found: 278[M+H]+.

1. extractionthe solution was extracted with DCM/MeOH (10/1, 3×400 mL)
2. washThe combined organic layers were washed with H2O (100 mL), and brine (100 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography (DCM:MeOH=15:1)