反应详情

To 20.0 g (74.3 mmol) (S)—N-(1-(4-bromophenyl)ethyl)acetamid (WO 2012/01107) in 300 mL THF are added dropwise 75.0 mL (187 mmol)N-butyllithium (2.5 M in THF) at −78° C. and stirred for 1 h. 10.0 mL (124 mmol) DMF are added dropwise to the mixture at −78° C. and stirred for 2 h. After that aq. NH4CI solution is added and extracted with EtOAc. The organic layer is dried over Na2SO4, filtered and concentrated by evaporation. The residue is purified by column chromatography (silica gel, MeOH:DCM).

1. stirringstirred for 2 h
2. extractionextracted with EtOAc
3. dry with materialThe organic layer is dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated by evaporation
6. customThe residue is purified by column chromatography (silica gel, MeOH:DCM)