1-[二氯甲基(乙氧基)磷酰基]氧乙烷

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 153.5 g (2.26 mol) of sodium ethylate in 800 ml of ethanol were added dropwise to a solution of 227.5 g (1.13 mol) of dichloromethane-phosphonic acid dichloride in 800 ml of toluene at 5°-10° C. The reaction mixture was subsequently stirred at 20° C. for five hours. It was then filtered, the filtrate was concentrated and the residue was subjected to fractional distillation. 195 g (78% of theory) of dichloromethane-phosphonic acid diethyl ester were obtained in the form of a colorless oil of boiling point 84° C./1 mbar. ##STR10## A suspension of 24.6 g (0.22 mol) of potassium tert.-butylate in 20 ml of dimethylformamide was added dropwise to a mixture of 48 g (0.22 mol) of dichloromethane-phosphonic acid diethyl ester and 34 g (0.2 mol) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester in 200 ml of tetrahydrofuran at -15° C. When the addition had ended, the reaction mixture was warmed to 20° C. and was stirred at this temperature for two hours. It was then filtered the filtrate was concentrated the residue was subjected to fractional distillation

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 153.5 g (2.26 mol) of sodium ethylate in 800 ml of ethanol were added dropwise, at 5°-10° C., to a solution of 227.5 g (1.13 mol) of dichloromethane-phosphonic acid dichloride in 800 ml of toluene. The mixture was subsequently stirred at 20° C. for 5 hours. It was then filtered, the filtrate was concentrated and the residue was subjected to fractional distillation. 195 g (78% of theory) of dichloromethane-phosphonic acid diethyl ester were obtained in the form of a colorless oil of boiling point 84° C./1 mbar. It was then filtered the filtrate was concentrated the residue was subjected to fractional distillation

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

实验步骤: A solution of 12.3 g (0.11 mol) of potassium tert.-butylate in 30 ml of dimethylformamide was added dropwise, under an inert gas atmosphere (nitrogen or argon) at -20° to -25° C., to a solution of 24 g (0.180 mol) of dichloromethane-phosphonic acid diethyl ester and 14 g (0.1 mol) of 2-acetyl-3,3-dimethylcyclopropanecarboxaldehyde in 100 ml of tetrahydrofuran. The mixture was subsequently stirred for 3 hours without cooling, 200 ml of water were added and extraction was carried out twice with 100 ml of methylene chloride. The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution and then with 3 times 50 ml of water, dried over sodium sulphate and evaporated in vacuo. 14.8 g (71% of theory) of 1-(2,2-dichlorovinyl)-2-acetyl-3,3-dimethylcyclopropane were obtained from the residue, by vacuum distillation, in the form of a pale yellow oil having a boiling point of 55°-57° C./0.3 mbar. without cooling extraction The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution with 3 times 50 ml of water, dried over sodium sulphate evaporated in vacuo

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 153.5 g (2.26 mol) of sodium ethylate in 800 ml of ethanol were added dropwise, at 5°-10° C., to a solution of 227.5 g (1.13 mol) of dichloromethane-phosphonic acid dichloride in 800 ml of toluene. The mixture was subsequently stirred at 20° C. for 5 hours. It was then filtered, the filtrate was concentrated and the residue was subjected to fractional distillation. 195 g (78% of theory) of dichloromethane-phosphonic acid diethyl ester were obtained in the form of a colorless oil of boiling point 84° C./1 mbar. It was then filtered the filtrate was concentrated the residue was subjected to fractional distillation

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

实验步骤: A solution of 12.3 g (0.11 mol) of potassium tert.-butylate in 30 ml of dimethylformamide was added dropwise, under an inert gas atmosphere (nitrogen or argon) at -20° to -25° C., to a solution of 24 g (0.180 mol) of dichloromethane-phosphonic acid diethyl ester and 14 g (0.1 mol) of 2-acetyl-3,3-dimethylcyclopropanecarboxaldehyde in 100 ml of tetrahydrofuran. The mixture was subsequently stirred for 3 hours without cooling, 200 ml of water were added and extraction was carried out twice with 100 ml of methylene chloride. The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution and then with 3 times 50 ml of water, dried over sodium sulphate and evaporated in vacuo. 14.8 g (71% of theory) of 1-(2,2-dichlorovinyl)-2-acetyl-3,3-dimethylcyclopropane were obtained from the residue, by vacuum distillation, in the form of a pale yellow oil having a boiling point of 55°-57° C./0.3 mbar. without cooling extraction The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution with 3 times 50 ml of water, dried over sodium sulphate evaporated in vacuo

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 153.5 g (2.26 mol) of sodium ethylate in 800 ml of ethanol were added dropwise to a solution of 227.5 g (1.13 mol) of dichloromethane-phosphonic acid dichloride in 800 ml of toluene at 5°-10° C. The reaction mixture was subsequently stirred at 20° C. for five hours. It was then filtered, the filtrate was concentrated and the residue was subjected to fractional distillation. 195 g (78% of theory) of dichloromethane-phosphonic acid diethyl ester were obtained in the form of a colorless oil of boiling point 84° C./1 mbar. ##STR10## A suspension of 24.6 g (0.22 mol) of potassium tert.-butylate in 20 ml of dimethylformamide was added dropwise to a mixture of 48 g (0.22 mol) of dichloromethane-phosphonic acid diethyl ester and 34 g (0.2 mol) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester in 200 ml of tetrahydrofuran at -15° C. When the addition had ended, the reaction mixture was warmed to 20° C. and was stirred at this temperature for two hours. It was then filtered the filtrate was concentrated the residue was subjected to fractional distillation

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 153.5 g (2.26 mol) of sodium ethylate in 800 ml of ethanol were added dropwise, at 5°-10° C., to a solution of 227.5 g (1.13 mol) of dichloromethane-phosphonic acid dichloride in 800 ml of toluene. The mixture was subsequently stirred at 20° C. for 5 hours. It was then filtered, the filtrate was concentrated and the residue was subjected to fractional distillation. 195 g (78% of theory) of dichloromethane-phosphonic acid diethyl ester were obtained in the form of a colorless oil of boiling point 84° C./1 mbar. It was then filtered the filtrate was concentrated the residue was subjected to fractional distillation

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

实验步骤: A solution of 12.3 g (0.11 mol) of potassium tert.-butylate in 30 ml of dimethylformamide was added dropwise, under an inert gas atmosphere (nitrogen or argon) at -20° to -25° C., to a solution of 24 g (0.180 mol) of dichloromethane-phosphonic acid diethyl ester and 14 g (0.1 mol) of 2-acetyl-3,3-dimethylcyclopropanecarboxaldehyde in 100 ml of tetrahydrofuran. The mixture was subsequently stirred for 3 hours without cooling, 200 ml of water were added and extraction was carried out twice with 100 ml of methylene chloride. The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution and then with 3 times 50 ml of water, dried over sodium sulphate and evaporated in vacuo. 14.8 g (71% of theory) of 1-(2,2-dichlorovinyl)-2-acetyl-3,3-dimethylcyclopropane were obtained from the residue, by vacuum distillation, in the form of a pale yellow oil having a boiling point of 55°-57° C./0.3 mbar. without cooling extraction The organic phase was washed with 50 ml of 10% strength sodium hydroxide solution with 3 times 50 ml of water, dried over sodium sulphate evaporated in vacuo