2-propan-2-ylidenecyclopentan-1-one

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

実験手順: Isoquinolinium perchlorate (2.3 g) and 2-isopropylidene cyclopentanone (1.5 g) in dimethylformamide (5 ml) were refluxed for 18 hours. The reaction mixture was cooled, diluted with methanol and filtered. Purification was effected by recrystallization from acetonitrile (norite). Yield 1.5 g, m.p. > 300°, The reaction mixture was cooled filtered Purification was effected by recrystallization from acetonitrile (norite)

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

実験手順: Isoquinolinium perchlorate (2.3 g) and 2-isopropylidene cyclopentanone (1.5 g) in dimethylformamide (5 ml) were refluxed for 18 hours. The reaction mixture was cooled, diluted with methanol and filtered. Purification was effected by recrystallization from acetonitrile (norite). Yield 1.5 g, m.p. > 300°, The reaction mixture was cooled filtered Purification was effected by recrystallization from acetonitrile (norite)

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

実験手順: Isoquinolinium perchlorate (2.3 g) and 2-isopropylidene cyclopentanone (1.5 g) in dimethylformamide (5 ml) were refluxed for 18 hours. The reaction mixture was cooled, diluted with methanol and filtered. Purification was effected by recrystallization from acetonitrile (norite). Yield 1.5 g, m.p. > 300°, The reaction mixture was cooled filtered Purification was effected by recrystallization from acetonitrile (norite)

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

実験手順: A mixture of 190 ml of acetone and 36.0 g of sodium hydroxide in 600 ml of water was treated with 60.0 g of cyclopentanone under stirring. After stirring for about 12 hours at about room temperature, the mixture was neutralized with 36% acetic acid and extracted with three 60 ml portions of ether. The combined extracts were dried over anhydrous magnesium sulfate and evaporated to give a residue. The residue was distilled to obtain 62.6 g of 2-(1-methylethylidene) cyclopentanone as a colorless liquid. The boiling point of this intermediate compound was determined to be 85°-88° C. at a pressure of 10 mm Hg. A subsequent Mannich reaction yielded the 2-Dimethylaminomethyl-5-(1-methylethylidene) cyclopentanone hydrochloride. The melting point of the product was determined to be 173°-175° C. After stirring for about 12 hours at about room temperature extracted with three 60 ml portions of ether The combined extracts were dried over anhydrous magnesium sulfate evaporated to give a residue The residue was distilled

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

実験手順: A mixture of 190 ml of acetone and 36.0 g of sodium hydroxide in 600 ml of water was treated with 60.0 g of cyclopentanone under stirring. After stirring for about 12 hours at about room temperature, the mixture was neutralized with 36% acetic acid and extracted with three 60 ml portions of ether. The combined extracts were dried over anhydrous magnesium sulfate and evaporated to give a residue. The residue was distilled to obtain 62.6 g of 2-(1-methylethylidene) cyclopentanone as a colorless liquid. The boiling point of this intermediate compound was determined to be 85°-88° C. at a pressure of 10 mm Hg. A subsequent Mannich reaction yielded the 2-Dimethylaminomethyl-5-(1-methylethylidene) cyclopentanone hydrochloride. The melting point of the product was determined to be 173°-175° C. After stirring for about 12 hours at about room temperature extracted with three 60 ml portions of ether The combined extracts were dried over anhydrous magnesium sulfate evaporated to give a residue The residue was distilled