反应详情

tert-butyl (2,6-dichloropyridin-4-yl)carbamate (460 mg, 1.75 mmol) from Step 1 of this example, ferric acetylacetonate (309 mg, 0.87 mmol) was added in THF:NMP (1:1, 17.4 mL), methyl magnesium bromide (3 mL [3M], 8.9 mmol) was added drop-wise and stirred for 15 min. The reaction was quenched with ice-cold ammonia chloride saturated solution (100 mL), extracted with ethyl acetate (100 mL), second wash with brine (50 mL). The organic phase was dried by magnesium sulfate and filtered through silica gel (1 inch deep), concentrated and purified by column chromatography through a 50 gram Biotage SNAP KP-Sil™ silica gel cartridge eluting with 10% ethyl acetate/hexanes to give the title compounds as a white solid.

1. customThe reaction was quenched with ice-cold ammonia chloride saturated solution (100 mL)
2. extractionextracted with ethyl acetate (100 mL)
3. washsecond wash with brine (50 mL)
4. dry with materialThe organic phase was dried by magnesium sulfate
5. filtrationfiltered through silica gel (1 inch deep)
6. concentrationconcentrated
7. custompurified by column chromatography through a 50 gram Biotage SNAP KP-Sil™ silica gel cartridge
8. washeluting with 10% ethyl acetate/hexanes