反应详情

N2-{[(1,1-dimethylethyl)oxy]carbonyl}-2-methylalaninamide (3.87 g, 19.13 mmol), Lawesson's reagent (7.74 g, 19.13 mmol) and tetrahydrofuran (THF) (100 mL) was heated to 50° C. for 3 hours. The reaction was concentrated, added 150 cc of EtOAc and washed with sat'd NaHCO3 (3×100 cc), water and brine. The EtOAc layer was concentrated and the residue was purified via chromatography on silica gel eluted Hex to 1:1 Hex/EtOAc to obtain the title compound (2.04 g, 48% yield).

1. concentrationThe reaction was concentrated
2. additionadded 150 cc of EtOAc
3. washwashed with sat'd NaHCO3 (3×100 cc), water and brine
4. concentrationThe EtOAc layer was concentrated
5. customthe residue was purified via chromatography on silica gel eluted Hex to 1:1 Hex/EtOAc