反应详情

温度

50 °C

5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum.

1. additionis added at 50° C.
2. distillationThe low-boiling components are distilled off under reduced pressure
3. extractionThe precipitated solid is extracted with a total of 130 ml of methylene chloride
4. dry with materialThe combined extracts are dried with magnesium sulfate
5. distillationthe methylene chloride is distilled off
6. customis sublimated at 60° C. in an oil pump vacuum