(2,6-dimethylphenyl) carbonochloridate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 70 ml of hydrogen fluoride and 200 ml of 1,1,2-trifluoro-1,2,2-trichloroethane were placed at 0° C. in a stainless steel autoclave and 100 g of 2,6-dimethylphenyl chloroformate were added dropwise. The autoclave was sealed and heated at a maximum temperature of 160° C. for 5 hours, the pressure of the gases formed being released at 30 bar. The reaction mixture was worked up as described in Example 9. 2,6-Dimethylfluorobenzene was obtained in a yield of 30% and 2,6-dimethylphenyl fluoroformate in a yield of 40%. The latter can be added to a new batch for the preparation of 2,6-dimethylfluorobenzene (see Example 15). were added dropwise The autoclave was sealed the pressure of the gases formed

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1.1 kg of anhydrous hydrogen fluoride were placed in a 3 l autoclave and the autoclave was sealed and heated to 130° C. At this temperature, 1 kg of 2,6-dimethylphenyl chloroformate was pumped in over a period of 3 hours, the pressure of the gases formed being released at 40 bar. Finally, the mixture was stirred for 1 hour at 130° C. The reaction mixture was then cooled and excess hydrogen fluoride was distilled off at 100 mbar. Further working-up of the reaction mixture was carried out as described in Example 9. 2,6-Dimethylfluorobenzene was obtained in a yield of 58.3%. the autoclave was sealed was pumped in over a period of 3 hours the pressure of the gases formed The reaction mixture was then cooled excess hydrogen fluoride was distilled off at 100 mbar

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 500 ml of anhydrous hydrogen fluoride were placed at 0° C. in a stainless steel laboratory autoclave and 150 g of 2,6-dimethylphenyl chloroformate were added dropwise. The autoclave was sealed and heated at a maximum temperature of 140° C. for 1.5 hours, the pressure of the gases formed being released at 26 bar. The reaction mixture was worked up as described in Example 9. 2,6-Dimethylfluorobenzene was obtained in a yield of 68.4%. were added dropwise The autoclave was sealed the pressure of the gases formed

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 500 ml of anhydrous hydrogen fluoride were placed at 0° C. in a stainless steel laboratory autoclave and 1000 g of 2,6-dimethylphenyl chloroformate were added dropwise. The autoclave was then sealed and heated at a maximum temperature of 110° C. for 2 hours, the pressure of the gases formed being released at 30 bar. The reaction mixture was worked up as described in Example 9. Distillation gave 2,6-dimethylfluorobenzene in a yield of 11% and 2,6-dimethylphenyl fluoroformate in a yield of 68%. The latter can be added to a new batch for the preparation of 2,6-dimethylfluorobenzene (see Example 15). were added dropwise The autoclave was then sealed the pressure of the gases formed Distillation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1000 ml of anhydrous hydrogen fluoride were placed at 0° C. in a stainless steel laboratory autoclave and 500 g of 2,6-dimethylphenyl chloroformate were added dropwise. The reaction was carried out and the reaction mixture worked up as described in Example 9. 2,6-Dimethylfluorobenzene was obtained in a yield of 51%. were added dropwise

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2000 ml of anhydrous hydrogen fluoride were placed at 0° in a stainless steel laboratory autoclave and 500 g of 2,6-dimethylphenyl chloroformate were added dropwise. The autoclave was then sealed and heated at a maximum temperature of 130° C. for 3 hours. The pressure of the gases evolved was released at 26 bar. The autoclave was then cooled to room temperature and the excess hydrogen fluoride was distilled off. The remaining reaction mixture was poured onto ice and the organic phase was separated off and distilled under vacuum. 2,6-Dimethylfluorobenzene was obtained in a yield of 69%. were added dropwise The autoclave was then sealed The autoclave was then cooled to room temperature the excess hydrogen fluoride was distilled off The remaining reaction mixture was poured onto ice the organic phase was separated off distilled under vacuum