2-chloro-N-(2,2-dimethoxyethyl)acetamide

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 105.1 grams (g) (1.0 moles) of aminoacetaldehyde dimethyl acetal, 80 g (1.0 moles) of a 50% aqueous solution of sodium hydroxide, and 200 ml dichloromethane are placed in a 1 liter flask fitted with a stirrer and thermometer. To this is added 113.0 g (1.0 moles) of chloroacetyl chloride dropwise with rapid stirring at 0°-10° C. After the addition is complete, the reaction is allowed to rise to room temperature and is stirred for 1 hour. Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water, followed by drying and evaporation to give 113.8 g (63% yield) of the title compound, m.p. 33°-36° C. are placed in a 1 liter flask fitted with a stirrer After the addition to rise to room temperature is stirred for 1 hour Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water by drying evaporation

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

実験手順: A mixture of 105.1 grams (g) (1.0 moles) of aminoacetaldehyde dimethyl acetal, 80 g (1.0 moles) of a 50% aqueous solution of sodium hydroxide, and 200 ml dichloromethane are placed in a 1 liter flask fitted with a stirrer and thermometer. To this is added 113.0 g (1.0 moles) of chloroacetyl chloride dropwise with rapid stirring at 0°-10° C. After the addition is complete, the reaction is allowed to rise to room temperature and is stirred for 1 hour. Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water, followed by drying and evaporation to give 113.8 g (63% yield) of the title compound, m.p. 33°-36° C. are placed in a 1 liter flask fitted with a stirrer After the addition to rise to room temperature is stirred for 1 hour Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water by drying evaporation

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

実験手順: A mixture of 105.1 grams (g) (1.0 moles) of aminoacetaldehyde dimethyl acetal, 80 g (1.0 moles) of a 50% aqueous solution of sodium hydroxide, and 200 ml dichloromethane are placed in a 1 liter flask fitted with a stirrer and thermometer. To this is added 113.0 g (1.0 moles) of chloroacetyl chloride dropwise with rapid stirring at 0°-10° C. After the addition is complete, the reaction is allowed to rise to room temperature and is stirred for 1 hour. Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water, followed by drying and evaporation to give 113.8 g (63% yield) of the title compound, m.p. 33°-36° C. are placed in a 1 liter flask fitted with a stirrer After the addition to rise to room temperature is stirred for 1 hour Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water by drying evaporation

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.2 grams; 0.1 mole), 1,3-propanediol (7.61 grams; 0.1 mole) and 10 drops of a solution of 1 gram of toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation head and condenser. The mixture was stirred and heated at about 120° C. for a period of about 1 hour while byproduct methanol was distilled off. The mixture was cooled to room temperature, sodium carbonate (2 grams) was added, and the slurry stirred for a period of about 1 hour. The slurry was filtered and the filtrate was stripped of solvent by mild warming under reduced pressure to yield the desired product N-(1,3-dioxan-2-ylmethyl)-2-chloracetamide as a residue. fitted with a mechanical stirrer thermometer, distillation head and condenser was distilled off The mixture was cooled to room temperature sodium carbonate (2 grams) was added the slurry stirred for a period of about 1 hour The slurry was filtered by mild warming under reduced pressure

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

実験手順: N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.1 grams; 0.10 mole) ethylene glycol (6.82 grams; 0.11 mole) and 10 drops of a solution of one gram of p-toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation heat and condenser. The mixture was stirred and heated to about 95° C. to 100° C. Byproduct methanol was distilled off. When no further methanol was evolved, the mixture was cooled to room temperature, sodium carbonate (2 grams) was added and the slurry was stirred for a period of about 1 hour. The slurry was then filtered and the filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide was obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when cooled, solidified. The solid had a melting point of 61° C.-63° C. fitted with a mechanical stirrer thermometer, distillation heat heated to about 95° C. to 100° C Byproduct methanol was distilled off sodium carbonate (2 grams) was added the slurry was stirred for a period of about 1 hour The slurry was then filtered the filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide was obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when cooled

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.2 grams; 0.1 mole), 1,3-propanediol (7.61 grams; 0.1 mole) and 10 drops of a solution of 1 gram of toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation head and condenser. The mixture was stirred and heated at about 120° C. for a period of about 1 hour while byproduct methanol was distilled off. The mixture was cooled to room temperature, sodium carbonate (2 grams) was added, and the slurry stirred for a period of about 1 hour. The slurry was filtered and the filtrate was stripped of solvent by mild warming under reduced pressure to yield the desired product N-(1,3-dioxan-2-ylmethyl)-2-chloracetamide as a residue. fitted with a mechanical stirrer thermometer, distillation head and condenser was distilled off The mixture was cooled to room temperature sodium carbonate (2 grams) was added the slurry stirred for a period of about 1 hour The slurry was filtered by mild warming under reduced pressure

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

実験手順: N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.1 grams; 0.10 mole) ethylene glycol (6.82 grams; 0.11 mole) and 10 drops of a solution of one gram of p-toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation head and condenser. The mixture was stirred and heated to about 95° C. to 100° C. Byproduct methanol was distilled off. When no further methanol was evolved, the mixture was cooled to room temperature, sodium carbonate (2 grams) was added and the slurry was stirred for a period of about 1 hour. The slurry was then filtered and the filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide was obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when cooled, solidfied. The solid had a melting point of 61° C.-63° C. fitted with a mechanical stirrer thermometer, distillation head and condenser heated to about 95° C. to 100° C Byproduct methanol was distilled off sodium carbonate (2 grams) was added the slurry was stirred for a period of about 1 hour The slurry was then filtered the filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide was obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when cooled

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

実験手順: A mixture of 105.1 grams (g) (1.0 moles) of aminoacetaldehyde dimethyl acetal, 80 g (1.0 moles) of a 50% aqueous solution of sodium hydroxide, and 200 ml dichloromethane are placed in a 1 liter flask fitted with a stirrer and thermometer. To this is added 113.0 g (1.0 moles) of chloroacetyl chloride dropwise with rapid stirring at 0°-10° C. After the addition is complete, the reaction is allowed to rise to room temperature and is stirred for 1 hour. Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water, followed by drying and evaporation to give 113.8 g (63% yield) of the title compound, m.p. 33°-36° C. are placed in a 1 liter flask fitted with a stirrer After the addition to rise to room temperature is stirred for 1 hour Next the mixture is washed with 100 ml water, 100 ml sodium carbonate solution and 100 ml water by drying evaporation