四碘化碳

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

实验步骤: Perfluoroneopentane is prepared from CI4 employing the apparatus described above. Five grams of carbon tetraiodide were placed in the Vycor container and the reactor was evacuated to 0.1 mm pressure. The Vycor container is located as in the position shown in the FIGURE. Hexafluoroethane was admitted to the reactor at a flow rate of 15 cc/min to maintain a 0.5 to 1 mm pressure during constant pumping. The discharge was initiated at 10 megahertz and 20 watts using a radio frequency generator. After eight hours the products were removed along with fluorocarbons from a -196°C trap downstream from the reactor. The products were separated from fluorocarbons by trap to trap distillation and purified using liquid nitrogen-cooled columns of a gas chromatograph. A 55 percent yield of the white solid CI(CF3)3 was obtained, which had a F19N.M.R. singlet -13.3 ppm from external trifluoroacetic acid. The mass spectrum contained a parent at 346 and a P-19 peak at 327. The infrared spectrum contained peaks at (1270) (960) and (725) cm-1. The elemental analysis was in agreement with the calculated values. The perfluoroneopentane C(CF3)4 was obtained in 25 percent yield and is a white solid melting at 72.5° to 73°C. The mass spectrum of the compound contains a p-19 at 269 while the F19N.M.R. consists of a singlet at -13.92 ppm from external trifluoroacetic acid. The infrared spectrum contains peaks at (9.80) (720) and 1190 cm-1. the reactor was evacuated to 0.1 mm pressure to maintain a 0.5 to 1 mm pressure After eight hours the products were removed along with fluorocarbons from a -196°C trap downstream from the reactor The products were separated from fluorocarbons by trap to trap distillation purified cooled columns of a gas chromatograph

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

实验步骤: (I4C): Fe powder (2.84 g, 50.9 mmol) was added to a solution of methyl 3-bromo-4-chloro-5-nitrobenzoate (5 g, 16.98 mmol) in AcOH (29.3 ml). The suspension was heated to 60° C. 1 h. The vessel was cooled to room temperature and then AcOH was removed via rotovap. The residue was placed in a 1 L beaker and was carefully neutralized with saturated sodium bicarbonate. The precipitate was removed via filtration through Celite and the filtrate was extracted with EtOAc. The organics were combined, washed with water and brine, and then dried over sodium sulfate. Filtration and concentration afforded methyl 3-amino-5-bromo-4-chlorobenzoate (4.19 g)) as a yellow solid. 1 h The vessel was cooled to room temperature AcOH was removed via rotovap The precipitate was removed via filtration through Celite the filtrate was extracted with EtOAc washed with water and brine dried over sodium sulfate Filtration and concentration

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

实验步骤: In a 200 ml stirring type autoclave were charged 30 mmols of aniline, 15 mmols of nitrobenzene, 50 ml of ethanol, 3 mmols of palladium chloride, 3 mmols of tetraiodomethane and 3 mmols of rubidium hydroxide. After the air inside the autoclave had been replaced with carbon monoxide, carbon monoxide was pressurized into the autoclave to 120 Kg/cm2, and the reaction was carried out at 180° C. for 5 hours with stirring. As the result of analysis of the reaction solution, the conversions of aniline and nitrobenzene were 21% and 29%, respectively, and 8 mmols of ethyl N-phenylcarbamate were obtained. with stirring As the result of analysis of the reaction solution

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

实验步骤: Perfluoroneopentane is prepared from CI4 employing the apparatus described above. Five grams of carbon tetraiodide were placed in the Vycorcontainer and the reactor was evacuated to 0.1 mm pressure. The Vycor container is located as in the position shown in the FIGURE. Hexafluoroethane was admitted to the reactor at a flow rate of 15 cc/min to maintain a 0.5 to 1 mm pressure during constant pumping. The discharge was initiated at 10 megahertz and 20 watts using a radio frequency generator. After eight hours the products were removed along with fluorocarbons from a -196° C trap downstream from the reactor. The products were separated from fluorocarbons by trap to trap distillation and purified using liquid nitrogen-cooled columns of a gas chromatograph. A 55% yield of the white solid CI(CF3)3 was obtained, which had a F19N.M.R. singlet -13.3 ppm from external trifluoroacetic acid. The mass spectrum contained a parent at 346 and a P-19 peak at 327. The infrared spectrum contained peaks at (1270) (960) and (725) cm-1. The elemental analysis was in agreement with the calculated values. The perfluoroneopentane C(CF3)4 was obtained in 25% yield and is a white solid melting at 72.5° to 73° C.The mass spectrum of the compound contains a P-19 at 269 while the F19N.M.R. consists of a singlet at -13.92 ppm from external trifluoroacetic acid. The infrared spectrum contains peaks at (9.80) (720) and 1190 cm-1. the reactor was evacuated to 0.1 mm pressure to maintain a 0.5 to 1 mm pressure After eight hours the products were removed along with fluorocarbons from a -196° C trap downstream from the reactor The products were separated from fluorocarbons by trap to trap distillation purified cooled columns of a gas chromatograph

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

实验步骤: (I4C): Fe powder (2.84 g, 50.9 mmol) was added to a solution of methyl 3-bromo-4-chloro-5-nitrobenzoate (5 g, 16.98 mmol) in AcOH (29.3 ml). The suspension was heated to 60° C. 1 h. The vessel was cooled to rt and then AcOH was removed via rotovap. The residue was placed in a 1 L beaker and was carefully neutralized with saturated sodium bicarbonate. The precipitate was removed via filtration through Celite and the filtrate was extracted with EtOAc. The organics were combined, washed with water and brine, then dried over sodium sulfate. Filtration and concentration afforded methyl 3-amino-5-bromo-4-chlorobenzoate (4.19 g)) as a yellow solid. 1 h The vessel was cooled to rt AcOH was removed via rotovap The precipitate was removed via filtration through Celite the filtrate was extracted with EtOAc washed with water and brine dried over sodium sulfate Filtration and concentration

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

实验步骤: Perfluoroneopentane is prepared from CI4 employing the apparatus described above. Five grams of carbon tetraiodide were placed in the Vycor container and the reactor was evacuated to 0.1 mm pressure. The Vycor container is located as in the position shown in the FIGURE. Hexafluoroethane was admitted to the reactor at a flow rate of 15 cc/min to maintain a 0.5 to 1 mm pressure during constant pumping. The discharge was initiated at 10 megahertz and 20 watts using a radio frequency generator. After eight hours the products were removed along with fluorocarbons from a -196°C trap downstream from the reactor. The products were separated from fluorocarbons by trap to trap distillation and purified using liquid nitrogen-cooled columns of a gas chromatograph. A 55 percent yield of the white solid CI(CF3)3 was obtained, which had a F19N.M.R. singlet -13.3 ppm from external trifluoroacetic acid. The mass spectrum contained a parent at 346 and a P-19 peak at 327. The infrared spectrum contained peaks at (1270) (960) and (725) cm-1. The elemental analysis was in agreement with the calculated values. The perfluoroneopentane C(CF3)4 was obtained in 25 percent yield and is a white solid melting at 72.5° to 73°C. The mass spectrum of the compound contains a p-19 at 269 while the F19N.M.R. consists of a singlet at -13.92 ppm from external trifluoroacetic acid. The infrared spectrum contains peaks at (9.80) (720) and 1190 cm-1. the reactor was evacuated to 0.1 mm pressure to maintain a 0.5 to 1 mm pressure After eight hours the products were removed along with fluorocarbons from a -196°C trap downstream from the reactor The products were separated from fluorocarbons by trap to trap distillation purified cooled columns of a gas chromatograph

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

实验步骤: (I4C): Fe powder (2.84 g, 50.9 mmol) was added to a solution of methyl 3-bromo-4-chloro-5-nitrobenzoate (5 g, 16.98 mmol) in AcOH (29.3 ml). The suspension was heated to 60° C. 1 h. The vessel was cooled to room temperature and then AcOH was removed via rotovap. The residue was placed in a 1 L beaker and was carefully neutralized with saturated sodium bicarbonate. The precipitate was removed via filtration through Celite and the filtrate was extracted with EtOAc. The organics were combined, washed with water and brine, and then dried over sodium sulfate. Filtration and concentration afforded methyl 3-amino-5-bromo-4-chlorobenzoate (4.19 g)) as a yellow solid. 1 h The vessel was cooled to room temperature AcOH was removed via rotovap The precipitate was removed via filtration through Celite the filtrate was extracted with EtOAc washed with water and brine dried over sodium sulfate Filtration and concentration