反应详情

Combine N,N′-dibenzyl-2-((R)-2-bromo-3-phenylpropionylamino)malonamide (0.49 g, 0.97 mmol) and thioacetic acid (0.172 mL, 2.42 mmol) in dimethylformamide (15 mL). Degas by repeated cycles of vacuum and filing with nitrogen. Add cesium carbonate (0.473 g, 1.45 mmol). After 18 hours, dilute the reaction mixture with water and extract twice with ethyl acetate. Combine the organic layers, extract with brine, dry over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 3/2 ethyl acetate/hexane to give the title compound (46%).

1. customDegas by repeated cycles of vacuum and filing with nitrogen
2. extractionextract twice with ethyl acetate
3. extractionextract with brine
4. dry with materialdry over Na2SO4
5. filtrationfilter
6. customevaporate in vacuo
7. customto give a residue