4,4,5,5-四氯-1,3-1,3-二氧戊环-2-酮[锗烷]

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C. shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

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: Broadly stated, the invention is a process for producing oxalyl chloride comprising: contacting ethylene carbonate with chlorine in a reaction vessel at a temperature in the range of about 70° to 100° C.; continuously circulating the above reaction mixture from the reaction vessel through an illuminated reaction zone of reduced cross-sectional area relative to that of the reaction vessel, and back into the reaction vessel to form tetrachloroethylene carbonate and hydrogen chloride; venting the hydrogen chloride from the reaction vessel; decomposing the tetrachloroethylene carbonate by heating tetrachloroethylene carbonate with a catalytic amount of a tertiary amine or amide to form oxalyl chloride and phosgene gas; and separating the phosgene gas from the oxalyl chloride.

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C. shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 360 mL "Hastelloy" C shaker tube was charged with 113 g (0.5 mole) of tetrachloroethylene carbonate, sealed under nitrogen, cooled in a dry ice acetone mixture, evacuated, flushed with nitrogen, reevacuated and charged with 18 g (0.9 mole) of hydrogen fluoride and 194 g (1.8 mole) of sulfur tetrafluoride. The tube was agitated for 10 hours at 200° C. The tube was next chilled in an ice-water bath and then slowly vented to remove the excess SF4 and HF. The product was dumped from the tube into wet ice and allowed to stand a day. The organic phase was separated from the aqueous phase in a polyethylene separatory funnel, then stirred with a 30% aqueous solution of potassium carbonate to neutralize free acid. The product was dried over potassium carbonate and distilled at a reduced pressure. It boils at 126° C. at atmospheric pressure. The best yield of 4,4,5,5-tetrachloro-2,2,-difluoro-1,3-dioxolane was 73%. Infrared and nuclear magnetic resonance (NMR) spectra support the chemical structure (4) of this dioxolane. sealed under nitrogen evacuated flushed with nitrogen The tube was next chilled in an ice-water bath to remove the excess SF4 and HF to stand a day The organic phase was separated from the aqueous phase in a polyethylene separatory funnel stirred with a 30% aqueous solution of potassium carbonate The product was dried over potassium carbonate distilled at a reduced pressure