反应详情

温度

92 °C

Combine 3-(2,2,3,3-tetrafluoropropoxy)tosylate (200 g, 0.664 mol), 3-hydroxybenzaldehyde (101.7 g, 0.833 mol), dimethylformamide (1.5 L) and powdered potassium carbonate (192 g). Heat under stirring at 92° C. for about 22 h. Cool the reaction mixture to 40° C., pour over ice-water and extract with ethyl acetate. Combine organic phases, wash with 1 N sodium hydroxide (1 L and 0.5 L) and then a solution of saturated sodium hydrogen carbonate, dry over magnesium sulfate, filter, evaporate to dryness to provide a oily residue. Distill the oily residue under reduced pressure in a Claisen flask to give a first fraction of the title compound: bp 108-110° C. under 0.4-0.5 mmHg and a second fraction at 110-111° C. under 0.4-0.5 mmHg.

1. temperatureHeat
2. temperatureCool the reaction mixture to 40° C.
3. extractionextract with ethyl acetate
4. washCombine organic phases, wash with 1 N sodium hydroxide (1 L and 0.5 L)
5. dry with materiala solution of saturated sodium hydrogen carbonate, dry over magnesium sulfate
6. filtrationfilter
7. customevaporate to dryness
8. customto provide a oily residue
9. distillationDistill the oily residue under reduced pressure in a Claisen flask