2-benzylidenecyclohexan-1-one

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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: To a solution of 29.6 g (0.1 mole) of 3,5-dimethoxy-4-hexyloxybenzoic acid hydrazide in 110 cm3 of anhydrous ethanol a solution of 18.6 g (0.1 mole) of 2-phenylmethylenecyclohexan-1-one in 50 cm3 of ethanol is added. The reaction mixture is boiled for one hour, cooled and filtered. 36.35 g (78.2%) of the named compound are obtained. M.p.: 158°-160° C. cooled filtered

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

実験手順: To a solution of 29.6 g (0.1 mole) of 3,5-dimethoxy-4-hexyloxybenzoic acid hydrazide in 110 cm3 of anhydrous ethanol a solution of 18.6 g (0.1 mole) of 2-phenylmethylenecyclohexan-1-one in 50 cm3 of ethanol is added. The reaction mixture is boiled for one hour, cooled and filtered. 36.35 g (78.2%) of the named compound are obtained. M.p.: 158°-160° C. cooled filtered

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

実験手順: To a solution of 37.2 g (0.2 moles) of 2-phenylmethylenecyclohexan-1-one in 200 ml of anhydrous ethanol a solution of 18.0 g (0.2 moles) of N-methoxycarbonyl hydrazine in 40 ml of anhydrous ethanol is added, under stirring. The reaction mixture is boiled for a short while, then cooled, clarified with activated carbon, filtered and the filtrate is cooled. The separated white crystals are filtered off and dried. 50.63 g of the desired compound are obtained. Yield: 98%. cooled filtered the filtrate is cooled The separated white crystals are filtered off dried

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

実験手順: To a solution of 29.6 g (0.1 mole) of 3,5-dimethoxy-4-hexyloxybenzoic acid hydrazide in 110 cm3 of anhydrous ethanol a solution of 18.6 g (0.1 mole) of 2-phenylmethylenecyclohexan-1-one in 50 cm3 of ethanol is added. The reaction mixture is boiled for one hour, cooled and filtered. 36.35 g (78.2%) of the named compound are obtained. M.p.: 158°-160° C. cooled filtered

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

実験手順: To a solution of 37.2 g (0.2 moles) of 2-phenylmethylenecyclohexan-1-one in 200 ml of anhydrous ethanol a solution of 18.0 g (0.2 moles) of N-methoxycarbonyl hydrazine in 40 ml of anhydrous ethanol is added, under stirring. The reaction mixture is boiled for a short while, then cooled, clarified with activated carbon, filtered and the filtrate is cooled. The separated white crystals are filtered off and dried. 50.63 g of the desired compound are obtained. Yield: 98%. cooled filtered the filtrate is cooled The separated white crystals are filtered off dried

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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: 43 g (0.23 mole) of 2-benzylidene-cyclohexanone obtained from Stage 2, and 21.6 g (0.23 mole) of dimethylammonium methylene chloride were stirred in 200 ml of dry acetonitrile at room temperature. After adding 0.2 ml of acetyl chloride the reaction mixture was stirred for a further 3 hours at room temperature, a colorless clear solution being formed. 200 ml of dry ether were then added dropwise to the reaction mixture, whereupon the hydrochloride crystallized out. 56.1 g (87% of theory) of colorless crystals were obtained. The base was released from the hydrochloride with dichloromethane/sodium hydroxide and, after drying the solution, the dichloromethane was removed by distillation. a colorless clear solution being formed crystallized out 56.1 g (87% of theory) of colorless crystals were obtained after drying the solution the dichloromethane was removed by distillation