2-diethoxyphosphorylethanol

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: by using 5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy-acetyl chloride and diethyl 2-hydroxyethylphosphonate there is obtained diethyl 2-[[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy]acetoxy]-ethylphosphonate, 1H-NMR (CDCl3, 400 MHz) 7.96 ppm (d, 1H), 7.80 ppm (d, 1H), 7.59 ppm (q, 1H), 7.21 ppm (d, 1H), 6.71 ppm (d, 1H), 6.52 ppm (q, 1H), 4.78 ppm (s, 2H), 4.45 ppm (m, 2H), 4.12 ppm (m, 4H), 2.17 ppm (m, 2H), 1.33 ppm (tt, 6H);

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

実験手順: by using 5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy-acetyl chloride and diethyl 2-hydroxyethylphosphonate there is obtained diethyl 2-[[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy]acetoxy]-ethylphosphonate, 1H-NMR (CDCl3, 400 MHz) 7.96 ppm (d, 1H), 7.80 ppm (d, 1H), 7.59 ppm (q, 1H), 7.21 ppm (d, 1H), 6.71 ppm (d, 1H), 6.52 ppm (q, 1H), 4.78 ppm (s, 2H), 4.45 ppm (m, 2H), 4.12 ppm (m, 4H), 2.17 ppm (m, 2H), 1.33 ppm (tt, 6H);

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

実験手順: by using 5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy-acetyl chloride and diethyl 2-hydroxyethylphosphonate there is obtained diethyl 2-[[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy]acetoxy]-ethylphosphonate, 1H-NMR (CDCl3, 400 MHz) 7.96 ppm (d, 1H), 7.80 ppm (d, 1H), 7.59 ppm (q, 1H), 7.21 ppm (d, 1H), 6.71 ppm (d, 1H), 6.52 ppm (q, 1H), 4.78 ppm (s, 2H), 4.45 ppm (m, 2H), 4.12 ppm (m, 4H), 2.17 ppm (m, 2H), 1.33 ppm (tt, 6H);

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:-50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.01 ml diethyl-(hydroxyethyl)-phosphonate are dissolved in 50 ml dichloromethane, combined with 4.42 ml of 2,6-lutidine and cooled to −50° C. Then a solution of 6 ml trifluoromethanesulphonic acid anhydride in 10 ml dichloromethane is slowly added dropwise. The mixture is allowed to come up to 0° C. within 1.5 hours and then diluted with 300 ml of cold diethyl ether. The precipitated solids are filtered off and the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo. The precipitated solids are filtered off the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution After drying with sodium sulphate the solvents

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

実験手順: 100 g of 2-acetoxyethane phosphonic acid diethyl ester are blended with 200 ml of methanol containing 1 wt.% of HCl and heated to 65°-70°C for 4 hours. A mixture of methyl acetate/methanol is removed continuously from the reaction mixture by distillation. Upon submitting the mixture of methyl acetate/methanol to gas chromatography no ethyl acetate at all and only traces of ethanol are found. The crude 2-hydroxyethanephosphonic acid diethyl ester is distilled under reduced pressure. 68 g of 2-hydroxyethane-phosphonic acid diethyl ester (b.p. 106°-109°C/0.1 torr) are obtained, corresponding to a yield of 83.5% of the theoretical. heated to 65°-70°C for 4 hours is removed continuously from the reaction mixture by distillation the mixture of methyl acetate/methanol to gas chromatography no ethyl acetate at all and only traces of ethanol The crude 2-hydroxyethanephosphonic acid diethyl ester is distilled under reduced pressure

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

実験手順: 100 g of 2-acetoxyethane phosphonic acid diethyl ester are heated to 80°C jointly with 200 ml of ethanol. To this solution are added dropwise within 5 hours 20 ml of ethanol containing 1 wt.% of H2SO4 while simultaneously removing by continuous distillation a mixture of ethylacetate and ethanol. The residue is submitted to distillation under reduced pressure. 64 g of 2-hydroxyethane-phosphonic acid diethyl ester are obtained, corresponding to a yield of 80% of the theoretical. while simultaneously removing by continuous distillation a mixture of ethylacetate and ethanol The residue is submitted to distillation under reduced pressure

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

実験手順: 100 g of 2-acetoxyethane phosphonic acid diethyl ester are blended with 200 ml of isobutyl alcohol containing 2 g of HCl and heated to 120°-150°C for 5 hours. A mixture of isobutyl acetate and isobutanol is removed continuously by distillation in the course of the reaction. By gas chromatography of the mixture of isobutyl acetate/isobutanol, no ethyl acetate and only traces of ethanol were found. 51 g of 2-hydroxyethane-phosphonic acid diethyl ester are obtained after distillation under reduced pressure, corresponding to a yield of 62% of the theoretical. heated to 120°-150°C for 5 hours is removed continuously by distillation in the course of the reaction By gas chromatography of the mixture of isobutyl acetate/isobutanol

反応条件: temp:-50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.01 ml diethyl-(hydroxyethyl)-phosphonate are dissolved in 50 ml dichloromethane, combined with 4.42 ml of 2,6-lutidine and cooled to −50° C. Then a solution of 6 ml trifluoromethanesulphonic acid anhydride in 10 ml dichloromethane is slowly added dropwise. Within 1.5 hours the mixture is allowed to come up to 0° C. and then diluted with 300 ml cold diethyl ether. Any solids precipitated are filtered off and the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo. to come up to 0° C. Any solids precipitated are filtered off the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution After drying with sodium sulphate the solvents

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

実験手順: by using 5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy-acetyl chloride and diethyl 2-hydroxyethylphosphonate there is obtained diethyl 2-[[5-(o-chloro-p-trifluoromethyl-phenoxy)-2-nitrophenoxy]acetoxy]-ethylphosphonate, 1H-NMR (CDCl3, 400 MHz) 7.96 ppm (d, 1H), 7.80 ppm (d, 1H), 7.59 ppm (q, 1H), 7.21 ppm (d, 1H), 6.71 ppm (d, 1H), 6.52 ppm (q, 1H), 4.78 ppm (s, 2H), 4.45 ppm (m, 2H), 4.12 ppm (m, 4H), 2.17 ppm (m, 2H), 1.33 ppm (tt, 6H);