反应详情

A solution of methyl 2-[(2-nitrophenyl)thio]benzoate (1.17 g, 4.04 mmol) in methanol (50 mL) was purged with nitrogen prior to the addition of 10% Pd/C catalyst (0.12 g). The mixture was again purged with nitrogen and then purged with hydrogen from a balloon. The mixture was stirred under hydrogen overnight. Additional amount of 10% Pd/C catalyst (0.24 g) was added, and the mixture was stirred under hydrogen overnight. The reaction mixture was filtered through a pad of celite, and the filtrate was concentrated. The residue was subjected to silica gel chromatography eluted with 100% DCM to provide methyl 2-[(2-aminophenyl)thio]benzoate as a yellow oil that crystallized over time. MS (ES, M+H+): 260.2

1. customThe mixture was again purged with nitrogen
2. custompurged with hydrogen from a balloon
3. additionAdditional amount of 10% Pd/C catalyst (0.24 g) was added
4. stirringthe mixture was stirred under hydrogen overnight
5. filtrationThe reaction mixture was filtered through a pad of celite
6. concentrationthe filtrate was concentrated
7. washeluted with 100% DCM