ethyl 3-(5-oxopyrrolidin-2-yl)propanoate

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: Twenty-eight grams of dihydro-1H-pyrrolizine-3,5(2H,6H)-dione (III) are dissolved in 100 g of ethyl alcohol and 0.2 ml of concentrated hydrochloric acid is added. The solution is heated at reflux for 104 hours. The mixture is cooled and excess ethyl alcohol is distilled at reduced pressure. The oil is dissolved in 1 l of anhydrous diethylether, 1 g of activated charcoal is added and the resulting suspension is filtered through filter aid. The filtrate is concentrated at reduced pressure and the resulting crystals are isolated by filtration. Recrystallization from carbon tetrachloride-petroleum ether yields 5-oxo-2-pyrrolidinepropanoic acid ethyl ester with a melting point of 60°-61° C. The solution is heated at reflux for 104 hours The mixture is cooled excess ethyl alcohol is distilled at reduced pressure The oil is dissolved in 1 l of anhydrous diethylether 1 g of activated charcoal is added the resulting suspension is filtered through filter aid The filtrate is concentrated at reduced pressure the resulting crystals are isolated by filtration Recrystallization from carbon tetrachloride-petroleum ether

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: Twenty-eight grams of dihydro-1H-pyrrolizine-3,5 (2H,6H)-dione (III) are dissolved in 100 g of ethyl alcohol and 0.2 ml of concentrated hydrochloric acid is added. The solution is heated at reflux for 104 hours. The mixture is cooled and excess ethyl alcohol is distilled at reduced pressure. The oil is dissolved in 1 l of anhydrous diethylether, 1 g of activated charcoal is added and the resulting suspension is filtered through filter aid. The filtrate is concentrated at reduced pressure and the resulting crystals are isolated by filtration. Recrystallization from carbon tetrachloride-petroleum ether yields 5-oxo-2-pyrrolidinepropanoic acid ethyl ester with a melting point of 60°-61° C. The solution is heated at reflux for 104 hours The mixture is cooled excess ethyl alcohol is distilled at reduced pressure The oil is dissolved in 1 l of anhydrous diethylether 1 g of activated charcoal is added the resulting suspension is filtered through filter aid The filtrate is concentrated at reduced pressure the resulting crystals are isolated by filtration Recrystallization from carbon tetrachloride-petroleum ether

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

実験手順: Twenty-eight grams of dihydro 1H-pyrrolizine-3,5 (2H, 6H) dione is dissolved in 100 g of ethyl alcohol and 0.2 ml of concentrated hydrochloric acid is added. The solution is heated at reflux for 104 hours. The mixture is cooled and excess ethyl alcohol is distilled at reduced pressure. The oil is dissolved in 1 l of anhydrous diethylether, 1 g of activated charcoal is added and the resulting suspension is filtered through filter aid. The filtrate is concentrated at reduced pressure and the resulting crystals are isolated by filtration. Recrystallization from carbon tetrachloridepetroleum ether yields 5-oxo-2-pyrrolidinepropanoic acid ethyl ester with a melting point of 60°-61° C. The solution is heated at reflux for 104 hours The mixture is cooled excess ethyl alcohol is distilled at reduced pressure The oil is dissolved in 1 l of anhydrous diethylether 1 g of activated charcoal is added the resulting suspension is filtered through filter aid The filtrate is concentrated at reduced pressure the resulting crystals are isolated by filtration Recrystallization from carbon tetrachloridepetroleum ether

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

実験手順: Twenty-eight grams of dihydro-1H-pyrrolizine-3,5(2H,6H)-dione (III) are dissolved in 100 g of ethyl alcohol and 0.2 ml of concentrated hydrochloric acid is added. The solution is heated at reflux for 104 hours. The mixture is cooled and excess ethyl alcohol is distilled at reduced pressure. The oil is dissolved in 1 l of anhydrous diethylether, 1 g of activated charcoal is added and the resulting suspension is filtered through filter aid. The filtrate is concentrated at reduced pressure and the resulting crystals are isolated by filtration. Recrystallization from carbon tetrachloride-petroleum ether yields 5-oxo-2-pyrrolidinepropanoic acid ethyl ester with a melting point of 60°-61° C. The solution is heated at reflux for 104 hours The mixture is cooled excess ethyl alcohol is distilled at reduced pressure The oil is dissolved in 1 l of anhydrous diethylether 1 g of activated charcoal is added the resulting suspension is filtered through filter aid The filtrate is concentrated at reduced pressure the resulting crystals are isolated by filtration Recrystallization from carbon tetrachloride-petroleum ether