1,1-dimethoxydecane

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

実験手順: Decanal dimethyl acetal was prepared by reacting 796 g decanal with 763.5 g trimethyl orthoformate in the presence of 1.97 g p-toluene sulfonic acid dissolved in 6.07 g methanol at a temperature of 45° C. for a period of time of 0.33 hours. The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution, and then with water; dried over anhydrous sodium sulfate; filtered through CELITE®/sodium sulfate and distilled at 92–98° C. at 4.36–4.97 mm Hg. Then, into a 2 liter reaction flask equipped with stirrer, thermometer, heating mantle, addition funnel, vacuum apparatus, and reflux condenser the following ingredients were added at 17° C.: The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution dried over anhydrous sodium sulfate filtered through CELITE®/sodium sulfate distilled at 92–98° C. at 4.36–4.97 mm Hg Then, into a 2 liter reaction flask equipped with stirrer thermometer, heating mantle, addition funnel, vacuum apparatus reflux condenser the following ingredients were added at 17° C.

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

実験手順: Decanal dimethyl acetal was prepared by reacting 796 g decanal with 763.5 g trimethyl orthoformate in the presence of 1.97 g p-toluene sulfonic acid dissolved in 6.07 g methanol at a temperature of 45° C. for a period of time of 0.33 hours. The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution, and then with water; dried over anhydrous sodium sulfate; filtered through CELITE®/sodium sulfate and distilled at 92–98° C. at 4.36–4.97 mm Hg. Then, into a 2 liter reaction flask equipped with stirrer, thermometer, heating mantle, addition funnel, vacuum apparatus, and reflux condenser the following ingredients were added at 17° C.: The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution dried over anhydrous sodium sulfate filtered through CELITE®/sodium sulfate distilled at 92–98° C. at 4.36–4.97 mm Hg Then, into a 2 liter reaction flask equipped with stirrer thermometer, heating mantle, addition funnel, vacuum apparatus reflux condenser the following ingredients were added at 17° C.

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

実験手順: 137.7 ml (1.5 mol) of POCl3 are added with ice cooling to 135 g (1.85 mol) of DMF, and the mixture is subsequently stirred at room temperature for 15 minutes. 202 g (1 mol) of decanal dimethyl acetal dissolved in 500 ml of DMF are then. added dropwise, and, after addition is complete, the mixture is stirred for about 3 further hours. 262.5 g (1 mol) of 4-benzoxybenzamidine are subsequently added, and the mixture is stirred for a further hour. 1.1 l of triethylamine are then slowly added, during which the temperature rises to about 70° C. In order to maintain stirrability, about 700 ml of DMF are added, and the triethylamine is subsequently removed by distillation at atmospheric pressure. The residue is poured into about 6 l of ice water. The precipitated product is washed with water, recrystallized from 2.5 1 of isobutanol, dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) until take-up of hydrogen ceases. The catalyst is filtered off with suction, and the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure. added dropwise after addition the mixture is stirred for about 3 further hours the mixture is stirred for a further hour rises to about 70° C are added the triethylamine is subsequently removed by distillation at atmospheric pressure The residue is poured into about 6 l of ice water The precipitated product is washed with water recrystallized from 2.5 1 of isobutanol dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) The catalyst is filtered off with suction the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure

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

実験手順: 137.7 ml (1.5 mol) of POCl3 are added with ice cooling to 135 g (1.85 mol) of DMF, and the mixture is subsequently stirred at room temperature for 15 minutes. 202 g (1 mol) of decanal dimethyl acetal dissolved in 500 ml of DMF are then. added dropwise, and, after addition is complete, the mixture is stirred for about 3 further hours. 262.5 g (1 mol) of 4-benzoxybenzamidine are subsequently added, and the mixture is stirred for a further hour. 1.1 l of triethylamine are then slowly added, during which the temperature rises to about 70° C. In order to maintain stirrability, about 700 ml of DMF are added, and the triethylamine is subsequently removed by distillation at atmospheric pressure. The residue is poured into about 6 l of ice water. The precipitated product is washed with water, recrystallized from 2.5 1 of isobutanol, dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) until take-up of hydrogen ceases. The catalyst is filtered off with suction, and the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure. added dropwise after addition the mixture is stirred for about 3 further hours the mixture is stirred for a further hour rises to about 70° C are added the triethylamine is subsequently removed by distillation at atmospheric pressure The residue is poured into about 6 l of ice water The precipitated product is washed with water recrystallized from 2.5 1 of isobutanol dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) The catalyst is filtered off with suction the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure

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

実験手順: 137.7 ml (1.5 mol) of POCl3 are added with ice cooling to 135 g (1.85 mol) of DMF, and the mixture is subsequently stirred at room temperature for 15 minutes. 202 g (1 mol) of decanal dimethyl acetal dissolved in 500 ml of DMF are then. added dropwise, and, after addition is complete, the mixture is stirred for about 3 further hours. 262.5 g (1 mol) of 4-benzoxybenzamidine are subsequently added, and the mixture is stirred for a further hour. 1.1 l of triethylamine are then slowly added, during which the temperature rises to about 70° C. In order to maintain stirrability, about 700 ml of DMF are added, and the triethylamine is subsequently removed by distillation at atmospheric pressure. The residue is poured into about 6 l of ice water. The precipitated product is washed with water, recrystallized from 2.5 1 of isobutanol, dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) until take-up of hydrogen ceases. The catalyst is filtered off with suction, and the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure. added dropwise after addition the mixture is stirred for about 3 further hours the mixture is stirred for a further hour rises to about 70° C are added the triethylamine is subsequently removed by distillation at atmospheric pressure The residue is poured into about 6 l of ice water The precipitated product is washed with water recrystallized from 2.5 1 of isobutanol dissolved in 1 l of ethyl acetate and hydrogenated at atmospheric pressure with addition of 10 g of Pd/C (10%) The catalyst is filtered off with suction the residue from evaporation of the filtrate is dried at 50° C. under reduced pressure

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

実験手順: Decanal dimethyl acetal was prepared by reacting 796 g decanal with 763.5 g trimethyl orthoformate in the presence of 1.97 g p-toluene sulfonic acid dissolved in 6.07 g methanol at a temperature of 45° C. for a period of time of 0.33 hours. The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution, and then with water; dried over anhydrous sodium sulfate; filtered through CELITE®/sodium sulfate and distilled at 92–98° C. at 4.36–4.97 mm Hg. Then, into a 2 liter reaction flask equipped with stirrer, thermometer, heating mantle, addition funnel, vacuum apparatus, and reflux condenser the following ingredients were added at 17° C.: The resulting product was washed with an aqueous 2.5% sodium bicarbonate solution dried over anhydrous sodium sulfate filtered through CELITE®/sodium sulfate distilled at 92–98° C. at 4.36–4.97 mm Hg Then, into a 2 liter reaction flask equipped with stirrer thermometer, heating mantle, addition funnel, vacuum apparatus reflux condenser the following ingredients were added at 17° C.