反应详情

1-Chloro-1-(4-chlorophenyl)-2-(N,N-diethylcarbamoyloxy)-2-methoxyiminoethane (16.6 grams; 0.05 mole), methyl ethyl ketone (100 ml), potassium O,O-diethyl phosphate (9.6 grams; 0.05 mole) and a few crystals of potassium iodide are charged into a glass reaction flask equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is then heated at reflux for a period of about 12 hours. After this time the reaction mixture is cooled to room temperature and is filtered to remove inorganic salts. The salts are washed with acetone and the washings combined with the filtrate. The resulting solution is stripped of solvents in a rotary evaporator. The remaining residue is dissolved in ether and the ether solution is washed with water and dried over anhydrous magnesium sulfate. The dried solution is filtered and stripped of ether to yield the desired product O-[1-(4-chlorophenyl)-2-(N,N-diethylcarbamoyloxy)-2-methoxyiminoethyl] O,O-diethyl phosphate.

1. customequipped with a mechanical stirrer
2. temperaturethermometer and reflux condenser
3. temperatureThe reaction mixture is then heated
4. temperatureat reflux for a period of about 12 hours
5. filtrationis filtered
6. customto remove inorganic salts
7. washThe salts are washed with acetone
8. customThe resulting solution is stripped of solvents in a rotary evaporator
9. dissolutionThe remaining residue is dissolved in ether
10. washthe ether solution is washed with water
11. dry with materialdried over anhydrous magnesium sulfate
12. filtrationThe dried solution is filtered