反应详情

To a solution of 2-methyl-1-nitro-2-thiopseudourea (430 mg, 3.19 mmol) in DMF (3 ml) was added Cs2CO3 (1.10 g, 3.38 mmol) and MeI (0.30 ml, 4.82 mmol) and the reaction stirred overnight. The mixture was then diluted with water (10 ml) and EtOAc (40 ml) and the organic layer washed with brine (3×15 ml), dried (Na2SO4) and concentrated. The resultant yellow oil was purified by column chromatography on silica gel (EtOAc/Hexanes, 1:1) to afford S-methyl N-nitro-N′-methylcarbamimidothioate (56 mg, 11%) as a white solid. 1H NMR (CDCl3) δ 2.52 (s, 3H), 3.12 (d, 3H, J=6 Hz), 10.05 (br s, 1H).

1. washthe organic layer washed with brine (3×15 ml)
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated
4. customThe resultant yellow oil was purified by column chromatography on silica gel (EtOAc/Hexanes, 1:1)