反应详情

After a reaction vessel which had been sufficiently dried inside by vacuum heating was replaced with dry nitrogen, 100 mL of a solution of 22.22 g (0.1 mol) of 2,2-difluoro-3-(methacryloyloxy)pentanoic acid in dichloromethane was added into the reaction vessel, and the mixture was cooled to an ice temperature. Thereto was added 100 mL of a solution of 22.70 g (0.11 mol) of DCC in dichloromethane over 10 min, and 0.61 g (5 mmol) of DMAP and 10.40 g (0.105 mol) of 2,2,2-trifluoroethanol were further added. Thereafter, the temperature of the reaction vessel was elevated to the room temperature, followed by stirring the mixture for 2 hrs, and 300 g of 1 N aqueous hydrochloric acid was added while intimately stirring. Subsequently, dichloromethane was separated by a separatory funnel, and the aqueous layer was extracted again with dichloromethane to obtain an extraction liquid. After the extraction liquid was combined with the dichloromethane layer and washed with 1 N aqueous hydrochloric acid, the solvent of the dichloromethane layer was distilled off with an evaporator, followed by purification by column chromatography to give 21.60 g of 2,2,2-trifluoroethyl-2,2-difluoro-3-(methacryloyloxy)pentanoate (M-5) (yield: 71%).

1. customAfter a reaction vessel which had been sufficiently dried inside by vacuum
2. temperatureheating
3. additionwas added into the reaction vessel
4. customwas elevated to the room temperature
5. stirringwhile intimately stirring
6. customSubsequently, dichloromethane was separated by a separatory funnel
7. extractionthe aqueous layer was extracted again with dichloromethane
8. customto obtain
9. extractionan extraction liquid
10. extractionAfter the extraction liquid
11. washwashed with 1 N aqueous hydrochloric acid
12. distillationthe solvent of the dichloromethane layer was distilled off with an evaporator
13. customfollowed by purification by column chromatography