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. Within 1.5 hours the mixture is allowed to come up to 0° C. and then diluted with 300 ml cold diethyl ether. Any solids precipitated 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. customto come up to 0° C.
2. customAny solids precipitated
3. filtrationare filtered off
4. washthe filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution
5. dry with materialAfter drying with sodium sulphate the solvents