1-溴-1,2,2-三氟乙烯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: In a 50 ml glass reactor equipped with PTFE valve and magnetic stirring, 2.4 g (0.02 moles) of ClCF2—CH2—OH, 5 ml of tert-butyl alcohol, 1.1 g (0.02 moli) of KOH and 3.5 g of CF2═CFBr (0.022 moles) are fed. The reaction mixture is left under stirring at room temperature for three hours. The organic phase is then diluted with water, separated, washed twice with slightly acid water by HCl and anhydrified. 5 g of a mixture having the following composition: 89% ClCF2—CH2—O—CF2CFHBr and 11% CF2═CH—O—CF2CFHBr are obtained. In a 50 ml glass reactor equipped with PTFE valve The reaction mixture is left separated washed twice with slightly acid water by HCl

反应条件: temp:-65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A -30° C. solution of bromotrifluoroethylene (7.15 g, 0.044 mol) in ether is treated with p-(chlorodimethylsilyl)phenetole (9.54 g, 0.044 mol), cooled to -65° C., treated dropwise with a 1.3M solution of sec-butyllithium in cyclohexane (34.2 mL, 0.044 mol) while maintaining the temperature below -60° C., stirred at -65° C. for 5 hours, stirred at room temperature overnight, cooled to 0° C., treated with dilute hydrochloric acid, and diluted with ether. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue which is distilled to give the title product as a clear liquid (7.66 g, bp 84°-92° C./0.8 mm Hg). while maintaining the temperature below -60° C. stirred at room temperature overnight cooled to 0° C. The organic phase is separated washed with brine dried over anhydrous magnesium sulfate concentrated in vacuo to obtain a residue which is distilled

反应条件: temp:-65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A -30° C. solution of bromotrifluoroethylene (7.15 g, 0.044 mol) in ether is treated with p-(chlorodimethylsilyl)phenetole (9.54 g, 0.044 mol), cooled to -65° C., treated dropwise with a 1.3M solution of sec-butyllithium in cyclohexane (34.2 mL, 0.044 mol) while maintaining the temperature below -60° C., stirred at -65° C. for 5 hours, stirred at room temperature overnight, cooled to 0° C., treated with dilute hydrochloric acid, and diluted with ether. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue which is distilled to give the title product as a clear liquid (7.66 g, bp 84°-92° C./0.8 mm Hg). while maintaining the temperature below -60° C. stirred at room temperature overnight cooled to 0° C. The organic phase is separated washed with brine dried over anhydrous magnesium sulfate concentrated in vacuo to obtain a residue which is distilled

反应条件: temp:-70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a multineck glass reactor equipped with: magnetic entrainment mechanical stirrer, reflux cooler, thermocouple, inner plunging pipes for introducing the reagents, and maintained at a temperature of -70° C., there were simultaneously fed--after having introduced 75 ml of dichlorodifluoromethane--0.75 l of bis(fluoroxy)difluoromethane at a flowrate of 0.375 l/h diluted with N2 (0.5 l/h) and bromotrifluoroethylene (5.4 g/h) for 2 hours. Into a multineck glass reactor equipped with: magnetic entrainment mechanical stirrer reflux cooler thermocouple, inner plunging pipes for introducing the reagents

反应条件: temp:-70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a multineck glass reactor equipped with: magnetic entrainment mechanical stirrer, reflux cooler, thermocouple, inner plunging pipes for introducing the reagents, and maintained at a temperature of -70° C., there were simultaneously fed--after having introduced 75 ml of dichlorodifluoromethane--0.75 l of bis(fluoroxy)difluoromethane at a flowrate of 0.375 l/h diluted with N2 (0.5 l/h) and bromotrifluoroethylene (5.4 g/h) for 2 hours. Into a multineck glass reactor equipped with: magnetic entrainment mechanical stirrer reflux cooler thermocouple, inner plunging pipes for introducing the reagents

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

实验步骤: In a 50 ml glass reactor equipped with PTFE valve and magnetic stirring, 2.4 g (0.02 moles) of ClCF2—CH2—OH, 5 ml of tert-butyl alcohol, 1.1 g (0.02 moli) of KOH and 3.5 g of CF2═CFBr (0.022 moles) are fed. The reaction mixture is left under stirring at room temperature for three hours. The organic phase is then diluted with water, separated, washed twice with slightly acid water by HCl and anhydrified. 5 g of a mixture having the following composition: 89% ClCF2—CH2—O—CF2CFHBr and 11% CF2═CH—O—CF2CFHBr are obtained. In a 50 ml glass reactor equipped with PTFE valve The reaction mixture is left separated washed twice with slightly acid water by HCl

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

实验步骤: In a 50 ml glass reactor equipped with PTFE valve and magnetic stirring, 2.4 g (0.02 moles) of ClCF2—CH2—OH, 5 ml of tert-butyl alcohol, 1.1 g (0.02 moli) of KOH and 3.5 g of CF2═CFBr (0.022 moles) are fed. The reaction mixture is left under stirring at room temperature for three hours. The organic phase is then diluted with water, separated, washed twice with slightly acid water by HCl and anhydrified. 5 g of a mixture having the following composition: 89% ClCF2—CH2—O—CF2CFHBr and 11% CF2═CH—O—CF2CFHBr are obtained. In a 50 ml glass reactor equipped with PTFE valve The reaction mixture is left separated washed twice with slightly acid water by HCl

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:38.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of zinc dust (15.72 g) and bromotrifluoroethylene (48.34 g, 0.30 mol) in N,N-dimethylformamide is heated to 38° C. After stirring at 38° C. for several minutes, the reaction mixture temperature rises to 65° C. over 30 minutes. The reaction mixture is then stirred for 90 minutes and cooled to −5° C. Copper(I) bromide (34.5 g, 0.24 mol) is then added to the cooled mixture. The reaction mixture is stirred at room temperature for 1 hour, treated sequentially with 1-(1-bromo-2-methylpropyl)-4-chlorobenzene (18.56 g, 0.075 mol) and limonene (5 drops), stirred at 49° C. overnight, cooled, and diluted with saturated ammonium chloride solution (400 mL) and concentrated ammonia solution (100 mL). The resultant aqueous mixture is extracted with hexanes. The combined organic extracts are washed sequentially with water, 10% hydrochloric acid, water, saturated sodium hydrogen carbonate solution and water, dried over anhydrous sodium sulfate, and concentrated in vacuo to obtain an oil. Column chromatography of the oil using silica gel and hexanes gives the title product as an oil (5.54 g) which is identified by NMR spectral analyses. The reaction mixture is then stirred for 90 minutes cooled to −5° C The reaction mixture is stirred at room temperature for 1 hour stirred at 49° C. overnight cooled The resultant aqueous mixture is extracted with hexanes The combined organic extracts are washed sequentially with water, 10% hydrochloric acid, water, saturated sodium hydrogen carbonate solution and water dried over anhydrous sodium sulfate concentrated in vacuo to obtain an oil

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Bromotrifluoroethylene (41.5 g, 257 mmol) was distilled (dry ice condenser) into a flask containing zinc (13.6 g, 208 mmol) and N,N-dimethylformamide (153 ml), and the resulting mixture was heated at approximately 60° C. for two hours. The reaction mixture was purged with nitrogen for one hour, cooled to −8° C., treated with cuprous bromide (29.83 g, 208 mmol), and stirred for 30 minutes without external cooling. 3-(4-chlorophenyl)-3-bromopropyl methyl ether (17.06 g, 64.7 mmol) in N,N-dimethylformamide (10 ml) was added followed by limonene (5 drops), and the resulting mixture was heated at 50° C. for 8 hours. The cooled reaction mixture was quenched with aqueous ammonium chloride and thoroughly extracted with hexane. The combined organic extracts were dried over anhydrous sodium sulfate and concentrated in vacuo to a brown oil (10.76 g). Chromatography on silica gel eluting with methylene chloride:hexane (1:9) afforded the title compound as a yellow oil (2.25 g), which was characterized by IR, 1HNMR and mass spectral analysis. The reaction mixture was purged with nitrogen for one hour cooled to −8° C. the resulting mixture was heated at 50° C. for 8 hours The cooled reaction mixture was quenched with aqueous ammonium chloride thoroughly extracted with hexane The combined organic extracts were dried over anhydrous sodium sulfate concentrated in vacuo to a brown oil (10.76 g)