反应详情

温度

25 °C

In a dry flask under argon was placed a solution of (3,4-dichloro-phenyl)-(4-toluenesulfonylhydrazono)-acetic acid methyl ester (1.45 g, 3.61 mmol) in dichloromethane (20 mL) containing triethylamine (0.55 mL, 3.97 mmol) at 25° C. The bright yellow solution was then stirred at 25° C. for 1 h, then the solvent was removed in vacuo to yield a bright yellow solid. The product was purified by flash chromatography (Merck Silica gel 60, 230-400 mesh, 7/1/0.5 hexanes/dichloromethane/methanol) to furnish diazo-(3,4-dichloro-phenyl)-acetic acid methyl ester (814 mg, 92% yield) as a bright yellowish orange solid: EI-HRMS m/e calcd for C9H6Cl2N2O2 (M+) 243.9806, found 243.9800.

1. customIn a dry flask under argon was placed
2. customthe solvent was removed in vacuo
3. customto yield a bright yellow solid
4. customThe product was purified by flash chromatography (Merck Silica gel 60, 230-400 mesh, 7/1/0.5 hexanes/dichloromethane/methanol)