Diethyl (trichloromethyl)phosphonate

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:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 25.5 g (0.1 mole) of trichloromethanephosphonic acid diethyl ester and 17.2 g (0.1 mole) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was added dropwise to 9.6 g of activated magnesium filings in 100 ml of dimethylformamide in a manner such that the reaction temperature did not exceed 60° C. When the exothermic reaction had ended, the reaction mixture was allowed to cool to room temperature. It was then filtered. 200 ml of water were added to the filtrate; this solution was extracted twice with 100 ml of methylene chloride each time. The combined methylene chloride extracts were dried over sodium sulphate and filtered. The filtrate was distilled. 3-(2,2-Dichloro-vinyl)-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was obtained in a yield of 60% of theory. did not exceed 60° C When the exothermic reaction It was then filtered 200 ml of water were added to the filtrate this solution was extracted twice with 100 ml of methylene chloride each time The combined methylene chloride extracts were dried over sodium sulphate filtered The filtrate was distilled

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

実験手順: A mixture of 25.5 g (0.1 mole) of trichloromethanephosphonic acid diethyl ester and 17.2 g (0.1 mole) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was added dropwise to 9.6 g of activated magnesium filings in 100 ml of dimethylformamide in a manner such that the reaction temperature did not exceed 60° C. When the exothermic reaction had ended, the reaction mixture was allowed to cool to room temperature. It was then filtered. 200 ml of water were added to the filtrate; this solution was extracted twice with 100 ml of methylene chloride each time. The combined methylene chloride extracts were dried over sodium sulphate and filtered. The filtrate was distilled. 3-(2,2-Dichloro-vinyl)-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was obtained in a yield of 60% of theory. did not exceed 60° C When the exothermic reaction It was then filtered 200 ml of water were added to the filtrate this solution was extracted twice with 100 ml of methylene chloride each time The combined methylene chloride extracts were dried over sodium sulphate filtered The filtrate was distilled

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

実験手順: A mixture of 25.5 g (0.1 mole) of trichloromethanephosphonic acid diethyl ester and 17.2 g (0.1 mole) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was added dropwise to 9.6 g of activated magnesium filings in 100 ml of dimethylformamide in a manner such that the reaction temperature did not exceed 60° C. When the exothermic reaction had ended, the reaction mixture was allowed to cool to room temperature. It was then filtered. 200 ml of water were added to the filtrate; this solution was extracted twice with 100 ml of methylene chloride each time. The combined methylene chloride extracts were dried over sodium sulphate and filtered. The filtrate was distilled. 3-(2,2-Dichloro-vinyl)-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was obtained in a yield of 60% of theory. did not exceed 60° C When the exothermic reaction It was then filtered 200 ml of water were added to the filtrate this solution was extracted twice with 100 ml of methylene chloride each time The combined methylene chloride extracts were dried over sodium sulphate filtered The filtrate was distilled

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 16.3 g (0.1 mole) of tris-dimethylaminophosphine were added dropwise to a mixture of 25.5 g (0.1 mole) of trichloromethanephosphonic acid diethyl ester and 17.2 g (0.1 mole) of 3-formyl-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester at a temperature of 40° C. The reaction mixture was then warmed to 90° C. for 3 to 4 hours. It was subsequently cooled and poured into 200 ml of water. This suspension was extracted twice with 100 ml of methylene chloride each time. The combined extracts were dried over sodium sulphate and then concentrated. 3-(2,2-Dichloro-vinyl)-2,2-dimethyl-cyclopropane-1-carboxylic acid ethyl ester was obtained in a yield of 88% of theory. It was subsequently cooled This suspension was extracted twice with 100 ml of methylene chloride each time The combined extracts were dried over sodium sulphate concentrated