反应详情

温度

23 °C

A suspension of 2,2-dimethyl-6-(3,3,3-trifluoro-2,2-dihydroxy-propyl)-[1,3]dioxin-4-one (example C.22 step 1) (70 g, 273 mmol) in toluene (500 mL) was placed in a preheated (135° C.) oilbath, needed 10 min to reflux, then was refluxed for 25 min while distilling off about 150 mL of solvent. The hot solution was concentrated in vacuum to about 300 mL, some heptane was added, cooled to 23° C., filtered the precipitate off, washed with little cold toluene and dried in HV to give the title compound a light yellow solid (17.93 g, 36%). MS (ISN) 179.1 [(M−H)−].

1. customwas placed in a preheated (135° C.) oilbath
2. temperatureto reflux
3. temperaturewas refluxed for 25 min
4. distillationwhile distilling off about 150 mL of solvent
5. concentrationThe hot solution was concentrated in vacuum to about 300 mL
6. additionsome heptane was added
7. filtrationfiltered the precipitate off,
8. washwashed with little cold toluene
9. customdried in HV