反应详情

4-Hydroxyxanthen-9-one (0.01 mole), acetonitrile (25 ml) and potassium carbonate (0.01 mole) are charged into a glass reaction vessel fitted with a mechanical stirrer and thermometer. O-Ethyl (2,4,6-trichlorophenyl)phosphonochloridate (0.01 mole) in acetonitrile (6 ml) is added dropwise, with stirring, at room temperature. The reaction mixture is stirred for a period of about 48 hours at a temperature of from about 35° C. to 50° C. It is then cooled to room temperature and filtered. Solvent is stripped from the filtrate using a rotary evaporator (70° C., 15 mm Hg). The devolatilized residue is redissolved in 1/1 v/v chloroform/cyclohexane (25 ml). This solution is then slurried with silica gel (2 grams) at room temperature for a period of about 2 hours, then filtered. Solvent is stripped from the filtrate using a rotary evaporator to yield the desired product O-ethyl O-(xanthen-9-one-4-yl) (2,4,6-trichlorophenyl)phosphonate.

1. customfitted with a mechanical stirrer
2. stirringThe reaction mixture is stirred for a period of about 48 hours at a temperature of from about 35° C. to 50° C
3. temperatureIt is then cooled to room temperature
4. filtrationfiltered
5. customa rotary evaporator (70° C., 15 mm Hg)
6. dissolutionThe devolatilized residue is redissolved in 1/1 v/v chloroform/cyclohexane (25 ml)
7. filtrationfiltered
8. customa rotary evaporator