反应详情

温度

160 °C

A mixture of 5-bromo-4-chloro-2-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methylpyrimidine (5.00 g, 17.0 mmol), cis-4-aminocyclohexanol hydrochloride (2.77 g, 18.3 mmol), and diisopropylethyl amine (8.69 mL, 49.9 mmol) in dimethylacetamide (60.0 mL) was heated at 160° C. in a sealed tube overnight. The reaction mixture was concentrated and the residue was purified by flash chromatography eluting with chloroform/methanol (0-3%). Combined fractions containing the desired product were concentrated. The resulting gum was dissolved in methyl tert-butyl ether (450 mL) and the solution was washed with 50% brine, dried (MgSO4), filtered and concentrated to afford the title compound as a orange foamy solid (5.53 g, 88%).

1. concentrationThe reaction mixture was concentrated
2. customthe residue was purified by flash chromatography
3. washeluting with chloroform/methanol (0-3%)
4. additionCombined fractions containing the desired product
5. concentrationwere concentrated
6. dissolutionThe resulting gum was dissolved in methyl tert-butyl ether (450 mL)
7. washthe solution was washed with 50% brine
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated