反应详情

温度

80 °C

To a solution of 5-bromo-2-methyl-pyridin-3-ylamine (Stage 75.1.4, 400 mg, 2.13 mmol) in isopropanol (33 ml) were added 4 M HCl in dioxane (0.535 ml, 2.13 mmol) and isoamyl nitrite (1.25 g, 10.7 mmol). The reaction mixture was heated at 80° C. for 2.5 h, before being evaporated to dryness. The residue was dissolved in EtOAc and washed with saturated aqueous NaHCO3. The aqueous layer was extracted with EtOAc and the combined organic layers were dried over Na2SO4, filtered and evaporated. The residue was dry loaded on silica gel and purified by MPLC (heptane/EtOAc 0% to 30%) to give the title compound as an orange oil (HPLC: tR 2.47 min (Method A); M+H=230, 232 MS-ES).

1. custombefore being evaporated to dryness
2. dissolutionThe residue was dissolved in EtOAc
3. washwashed with saturated aqueous NaHCO3
4. extractionThe aqueous layer was extracted with EtOAc
5. dry with materialthe combined organic layers were dried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. customThe residue was dry
9. custompurified by MPLC (heptane/EtOAc 0% to 30%)