N-benzyl-2-chloro-N-propan-2-ylacetamide

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

実験手順: A solution of 7.66 g of the N-benzyl-2-chloro-N-isopropylacetamide in 20 ml of dry diethyl ether was added dropwise to a suspension of 1.29 g of lithium aluminum hydride in 300 ml of dry diethyl ether with stirring under ice-cooling, and the mixture was heated under reflux for 4 hours. After the reaction mixture was cooled, and to the cooled reaction mixture was added dropwise water with stirring under ice-cooling. Insoluble materials were filtered off. The filtrate was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (eluent: chloroform) to obtain 3.61 g of 2-(N-isopropylbenzylamino)ethyl chloride in an oil. cooling the mixture was heated under reflux for 4 hours After the reaction mixture was cooled to the cooled reaction mixture with stirring under ice- cooling Insoluble materials were filtered off The filtrate was dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was purified with silica gel column chromatography (eluent: chloroform)

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

実験手順: To a solution of 5.00 g of N-isopropylbenzylamine and 3.74 g of triethylamine in 60 ml of dry dichloromethane was added dropwise 3.84 g of chloroacetyl chloride with stirring under ice-cooling. The mixture was heated under reflux for 2 hours. After cooling, the reaction mixture was successively washed with water, a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 7.67 g of N-benzyl-2-chloro-N-isopropylacetamide in an oil. cooling The mixture was heated under reflux for 2 hours After cooling the reaction mixture was successively washed with water a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: To a solution of 5.00 g of N-isopropylbenzylamine and 3.74 g of triethylamine in 60 ml of dry dichloromethane was added dropwise 3.84 g of chloroacetyl chloride with stirring under ice-cooling. The mixture was heated under reflux for 2 hours. After cooling, the reaction mixture was successively washed with water, a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 7.67 g of N-benzyl-2-chloro-N-isopropylacetamide in an oil. cooling The mixture was heated under reflux for 2 hours After cooling the reaction mixture was successively washed with water a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: A solution of 7.66 g of the N-benzyl-2-chloro-N-isopropylacetamide in 20 ml of dry diethyl ether was added dropwise to a suspension of 1.29 g of lithium aluminum hydride in 300 ml of dry diethyl ether with stirring under ice-cooling, and the mixture was heated under reflux for 4 hours. After the reaction mixture was cooled, and to the cooled reaction mixture was added dropwise water with stirring under ice-cooling. Insoluble materials were filtered off. The filtrate was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (eluent: chloroform) to obtain 3.61 g of 2-(N-isopropylbenzylamino)ethyl chloride in an oil. cooling the mixture was heated under reflux for 4 hours After the reaction mixture was cooled to the cooled reaction mixture with stirring under ice- cooling Insoluble materials were filtered off The filtrate was dried over anhydrous magnesium sulfate concentrated under reduced pressure The residue was purified with silica gel column chromatography (eluent: chloroform)

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

実験手順: To a solution of 5.00 g of N-isopropylbenzylamine and 3.74 g of triethylamine in 60 ml of dry dichloromethane was added dropwise 3.84 g of chloroacetyl chloride with stirring under ice-cooling. The mixture was heated under reflux for 2 hours. After cooling, the reaction mixture was successively washed with water, a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 7.67 g of N-benzyl-2-chloro-N-isopropylacetamide in an oil. cooling The mixture was heated under reflux for 2 hours After cooling the reaction mixture was successively washed with water a 10% hydrochloric acid and an aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate concentrated under reduced pressure