反应详情

To 3-{[tert-butyl(dimethyl)silyl]oxy}benzene-1,2-diamine (4.27 g, 17.9 mmol) is added diethoxymethyl acetate (8.7 g, 53.6 mmol), and the mixture is stirred at room temperature for 5 hours. The precipitated white solid is collected by filtration, and the filtrate is further stirred at room temperature for 12 hours. The precipitated white solid is collected by filtration, and washed with a small amount of hexane. The filtrate is concentrated under reduced pressure, ant the obtained residue is purified by silica gel column chromatography (ammonic chloroform) to give the title compound as white solid (1.89 g, yield: 43%).

1. filtrationThe precipitated white solid is collected by filtration
2. stirringthe filtrate is further stirred at room temperature for 12 hours
3. filtrationThe precipitated white solid is collected by filtration
4. washwashed with a small amount of hexane
5. concentrationThe filtrate is concentrated under reduced pressure, ant the obtained residue
6. customis purified by silica gel column chromatography (ammonic chloroform)