1-diethoxyphosphorylpropane

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

実験手順: 53 g of acrylonitrile are added dropwise under nitrogen at a reaction temperature of 70° C. to a mixture of 160 g of diethyl propanephosphonate in 100 g of n-propylmercaptan in the course of 2 hours. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation; the crude product is obtained in a yield of 173 g with a 95.4% purity, which corresponds to a theoretical yield of 94.4%. The boiling point of the product is 117°-118° C. at 0.027 mbar. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation

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

実験手順: 53 g of acrylonitrile are added dropwise under nitrogen at a reaction temperature of 70° C. to a mixture of 160 g of diethyl propanephosphonate in 100 g of n-propylmercaptan in the course of 2 hours. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation; the crude product is obtained in a yield of 173 g with a 95.4% purity, which corresponds to a theoretical yield of 94.4%. The boiling point of the product is 117°-118° C. at 0.027 mbar. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation

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

実験手順: 53 g of acrylonitrile are added dropwise under nitrogen at a reaction temperature of 70° C. to a mixture of 160 g of diethyl propanephosphonate in 100 g of n-propylmercaptan in the course of 2 hours. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation; the crude product is obtained in a yield of 173 g with a 95.4% purity, which corresponds to a theoretical yield of 94.4%. The boiling point of the product is 117°-118° C. at 0.027 mbar. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation

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

実験手順: 200 g of phosgene were passed into 1 mole of propane-phosphonic acid diethyl ester at 70°-80° C. The mixture was stirred at 70°-80° C. for 1 hour and a dry N2 stream was passed through the reaction mixture overnight at 50° C. The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor and crude propanephosphonic acid ethyl ester-chloride was obtained. This was rendered basic with absolute pyridine, dissolved in 300 ml of toluene and reacted with a mixture of 1.1 moles of pyridine and 1 mole of allyl alcohol at 20°-30° C. The mixture was allowed to after-react at 80° C. for 2 hours. The solution which was separated off from the hydrochloride by filtration was concentrated and distilled. was passed through the reaction mixture overnight at 50° C The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor

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

実験手順: 200 g of phosgene were passed into 1 mole of propane-phosphonic acid diethyl ester at 70°-80° C. The mixture was stirred at 70°-80° C. for 1 hour and a dry N2 stream was passed through the reaction mixture overnight at 50° C. The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor and crude propanephosphonic acid ethyl ester-chloride was obtained. This was rendered basic with absolute pyridine, dissolved in 300 ml of toluene and reacted with a mixture of 1.1 moles of pyridine and 1 mole of allyl alcohol at 20°-30° C. The mixture was allowed to after-react at 80° C. for 2 hours. The solution which was separated off from the hydrochloride by filtration was concentrated and distilled. was passed through the reaction mixture overnight at 50° C The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor

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

実験手順: 53 g of acrylonitrile are added dropwise under nitrogen at a reaction temperature of 70° C. to a mixture of 160 g of diethyl propanephosphonate in 100 g of n-propylmercaptan in the course of 2 hours. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation; the crude product is obtained in a yield of 173 g with a 95.4% purity, which corresponds to a theoretical yield of 94.4%. The boiling point of the product is 117°-118° C. at 0.027 mbar. After a further 3 hours the solvent (low-boiling solvent such as C3H7SC2H5 and excess C3H7SH) is removed by vacuum distillation

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

実験手順: 200 g of phosgene were passed into 1 mole of propane-phosphonic acid diethyl ester at 70°-80° C. The mixture was stirred at 70°-80° C. for 1 hour and a dry N2 stream was passed through the reaction mixture overnight at 50° C. The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor and crude propanephosphonic acid ethyl ester-chloride was obtained. This was rendered basic with absolute pyridine, dissolved in 300 ml of toluene and reacted with a mixture of 1.1 moles of pyridine and 1 mole of allyl alcohol at 20°-30° C. The mixture was allowed to after-react at 80° C. for 2 hours. The solution which was separated off from the hydrochloride by filtration was concentrated and distilled. was passed through the reaction mixture overnight at 50° C The mixture was completely degassed at 50° C. under a waterpump vacuum in a Rotavapor