反应详情

温度

-50 °C

5.01 ml diethyl-(hydroxyethyl)-phosphonate are dissolved in 50 ml dichloromethane, combined with 4.42 ml of 2,6-lutidine and cooled to −50° C. Then a solution of 6 ml trifluoromethanesulphonic acid anhydride in 10 ml dichloromethane is slowly added dropwise. The mixture is allowed to come up to 0° C. within 1.5 hours and then diluted with 300 ml of cold diethyl ether. The precipitated solids are filtered off and the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo.

1. filtrationThe precipitated solids are filtered off
2. washthe filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution
3. dry with materialAfter drying with sodium sulphate the solvents