5-chloro-2-ethoxybenzoyl chloride

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

実験手順: 10.5 g of 4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride were suspended in 40 ml of dioxane and 20 ml of acetone and the suspension was combined with 8 ml of pyridine. To this suspension, a solution of 10 g of 2-ethoxy-5-chloro-benzoyl chloride in a small amount of acetone was added dropwise, while stirring, and the whole was heated for 2 hours under reflux. After cooling, the mixture was concentrated under reduced pressure, combined with ice-water, filtered with suction, stirred with dilute hydrochloric acid and with a NaHCO3 solution and the resulting product was again filtered off with suction and recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid methyl ester obtained was found to melt at 110° C. the whole was heated for 2 hours under reflux After cooling the mixture was concentrated under reduced pressure filtered with suction stirred with dilute hydrochloric acid and with a NaHCO3 solution the resulting product was again filtered off with suction recrystallized from ethanol

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

実験手順: 10 g of 4-(2-aminoethyl)-benzoic acid hydrochloride were dissolved in 60 ml of 2 N-sodium hydroxide solution and, after addition of 75 ml of acetone, a solution of 11 g of 2-ethoxy-5-chloro-benzoylchloride in 20 ml of acetone was added dropwise, while stirring. Stirring was continued for 2 hours, the mixture was diluted with water, filtered and acidified with dilute hydrochloric acid. After filtration with suction, the product was recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid obtained was found to melt at 180° C. Stirring filtered After filtration with suction the product was recrystallized from ethanol

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

実験手順: 10.5 g of 4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride were suspended in 40 ml of dioxane and 20 ml of acetone and the suspension was combined with 8 ml of pyridine. To this suspension, a solution of 10 g of 2-ethoxy-5-chloro-benzoyl chloride in a small amount of acetone was added dropwise, while stirring, and the whole was heated for 2 hours under reflux. After cooling, the mixture was concentrated under reduced pressure, combined with ice-water, filtered with suction, stirred with dilute hydrochloric acid and with a NaHCO3 solution and the resulting product was again filtered off with suction and recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid methyl ester obtained was found to melt at 110° C. the whole was heated for 2 hours under reflux After cooling the mixture was concentrated under reduced pressure filtered with suction stirred with dilute hydrochloric acid and with a NaHCO3 solution the resulting product was again filtered off with suction recrystallized from ethanol

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

実験手順: 10 g of 4-(2-aminoethyl)-benzoic acid hydrochloride were dissolved in 60 ml of 2 N-sodium hydroxide solution and, after addition of 75 ml of acetone, a solution of 11 g of 2-ethoxy-5-chloro-benzoylchloride in 20 ml of acetone was added dropwise, while stirring. Stirring was continued for 2 hours, the mixture was diluted with water, filtered and acidified with dilute hydrochloric acid. After filtration with suction, the product was recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid obtained was found to melt at 180° C. Stirring filtered After filtration with suction the product was recrystallized from ethanol

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

実験手順: 10.5 g of 4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride were suspended in 40 ml of dioxane and 20 ml of acetone and the suspension was combined with 8 ml of pyridine. To this suspension, a solution of 10 g of 2-ethoxy-5-chloro-benzoyl chloride in a small amount of acetone was added dropwise, while stirring, and the whole was heated for 2 hours under reflux. After cooling, the mixture was concentrated under reduced pressure, combined with ice-water, filtered with suction, stirred with dilute hydrochloric acid and with a NaHCO3 solution and the resulting product was again filtered off with suction and recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid methyl ester obtained was found to melt at 110° C. the whole was heated for 2 hours under reflux After cooling the mixture was concentrated under reduced pressure filtered with suction stirred with dilute hydrochloric acid and with a NaHCO3 solution the resulting product was again filtered off with suction recrystallized from ethanol

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

実験手順: 10 g of 4-(2-aminoethyl)-benzoic acid hydrochloride were dissolved in 60 ml of 2 N-sodium hydroxide solution and, after addition of 75 ml of acetone, a solution of 11 g of 2-ethoxy-5-chloro-benzoylchloride in 20 ml of acetone was added dropwise, while stirring. Stirring was continued for 2 hours, the mixture was diluted with water, filtered and acidified with dilute hydrochloric acid. After filtration with suction, the product was recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid obtained was found to melt at 180° C. Stirring filtered After filtration with suction the product was recrystallized from ethanol