1,1,1,3,3,3-六氟-2-氯甲氧基丙烷

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 1 liter stainless steel autoclave (Parr) was charged with 127.3 g (2.19 mole) of potassium fluoride and 434.6 g (2.01 mole) of (CF3)2CHOCH2Cl. The autoclave was then sealed and the reaction mass heated at 185° C. for 19 hours, during which time a pressure of 280 psi developed. The reactor was then cooled, the contents treated with water and the organic material distilled to afford 241 g (1.21 mole) of (CF3)2CHOCH2F and 80 g (0.4 mole) of (CF3)2CHOCH2Cl, corresponding to a 60% conversion (75% yield). The structure of (CF3)2CHOCH2F (Sevoflurane), b.p. 56° C., may be confirmed by the following instrumental data: The autoclave was then sealed The reactor was then cooled the organic material distilled

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In an efficient fume hood, liquid hydrogen fluoride (85.1 g, 4.25 mol) was transferred into a 1 liter Teflon® reaction vessel chilled in a dry ice/acetone cold bath. The vessel was fitted with a dry ice condenser, thermocouple, and addition funnel and a portion of chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether (80.1 g) was added. A solution of diisopropylethylamine (249.0 g, 1.93 mol) in chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether (271.0 g) was slowly added while maintaining the internal temperature in the range of -5°to 10° C. After completing the addition, the mixture was transferred to a 2 liter glass boiling flask and the Teflon® vessel was rinsed out with a solution of diisopropylethylamine (307.0 g, 2.38 mol) in chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether (180.0 g) which was also transferred to the glass flask. An additional 850 g of chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether was added to the reaction flask to bring the total to 1381.1 g (6.38 mol). This mixture was heated at reflux for 16 hours. After cooling to ambient temperature, water (700 mL) was added to the reaction mixture and, after vigorous shaking, the resultant layers were separated. The lower organic layer was further washed with 700 mL of dilute hydrochloric acid (35 mL of 12 N HCl in 665 mL of water). The organic layer (1259.7 g) was analyzed by NMR and gas chromatography and was shown to consist of 63.6% fluoromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether (sevoflurane) and 35.4% recovered chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether, giving a 95% yield of sevoflurane based on starting material consumed. chilled in a dry ice/acetone cold bath The vessel was fitted with a dry ice condenser thermocouple, and addition funnel the addition This mixture was heated at reflux for 16 hours After cooling to ambient temperature after vigorous shaking, the resultant layers were separated The lower organic layer was further washed with 700 mL of dilute hydrochloric acid (35 mL of 12 N HCl in 665 mL of water) recovered chloromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether