反应详情

41.7 ml of 1.6M n-butyllithium in hexane and 7.7 g of TMEDA are added, under nitrogen, to 5 g of 5-(N-Boc-amino)-2-methoxypyridine, at −60° C. The medium turns yellow. The mixture is left stirring for 4 hours, allowing the temperature to return to −10° C., and a pale yellow. precipitate forms. The mixture is recooled to −40° C. and 4.7 g of methyl iodide are then added. The medium is allowed to return to RT and is then poured into water and extracted with EtOAc, and the extracts are dried and evaporated. The residue is chromatographed on silica, eluting with cyclohexane/EtOAc (85/15; v/v).

1. waitThe mixture is left
2. customto return to −10° C.
3. customis recooled to −40° C.
4. customto return to RT
5. extractionextracted with EtOAc
6. customthe extracts are dried
7. customevaporated
8. customThe residue is chromatographed on silica
9. washeluting with cyclohexane/EtOAc (85/15; v/v)