ethyl N-methyl-N-piperidin-4-ylcarbamate

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: 4 g of the compound obtained in Stage H, 2.24 g of the compound obtained in Stage B of Example 6 and 1.7 ml of triethanolamine are refluxed in 40 ml of toluene for 24 hours. The reaction mixture is concentrated, taken up in ethyl acetate, washed with water and then extracted with 1 N hydrochloric acid, and the extract is rendered basic with concentrated sodium hydroxide solution and extracted with methylene chloride. The extract is dried to yield ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate. 23.5 ml of a 2% solution of fumaric acid in ethanol are added to yield the desired salt. The reaction mixture is concentrated washed with water extracted with 1 N hydrochloric acid extracted with methylene chloride The extract is dried

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

実験手順: 4 g of the compound obtained in Stage H, 2.24 g of the compound obtained in Stage B of Example 6 and 1.7 ml of triethanolamine are refluxed in 40 ml of toluene for 24 hours. The reaction mixture is concentrated, taken up in ethyl acetate, washed with water and then extracted with 1 N hydrochloric acid, and the extract is rendered basic with concentrated sodium hydroxide solution and extracted with methylene chloride. The extract is dried to yield ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate. 23.5 ml of a 2% solution of fumaric acid in ethanol are added to yield the desired salt. The reaction mixture is concentrated washed with water extracted with 1 N hydrochloric acid extracted with methylene chloride The extract is dried

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

実験手順: 49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound. are hydrogenated at 50° C. under 5 Kg The catalyst is filtered off the filtrate is evaporated recovered with diethyl ether The ethereal phase is dried evaporated

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

実験手順: 49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound. are hydrogenated at 50° C. under 5 Kg The catalyst is filtered off the filtrate is evaporated recovered with diethyl ether The ethereal phase is dried evaporated

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

実験手順: 4 g of the compound obtained in Stage H, 2.24 g of the compound obtained in Stage B of Example 6 and 1.7 ml of triethanolamine are refluxed in 40 ml of toluene for 24 hours. The reaction mixture is concentrated, taken up in ethyl acetate, washed with water and then extracted with 1 N hydrochloric acid, and the extract is rendered basic with concentrated sodium hydroxide solution and extracted with methylene chloride. The extract is dried to yield ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate. 23.5 ml of a 2% solution of fumaric acid in ethanol are added to yield the desired salt. The reaction mixture is concentrated washed with water extracted with 1 N hydrochloric acid extracted with methylene chloride The extract is dried

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

実験手順: 49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound. are hydrogenated at 50° C. under 5 Kg The catalyst is filtered off the filtrate is evaporated recovered with diethyl ether The ethereal phase is dried evaporated

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: 49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound. are hydrogenated at 50° C. under 5 Kg The catalyst is filtered off the filtrate is evaporated recovered with diethyl ether The ethereal phase is dried evaporated

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

実験手順: 4 g of the compound obtained in Stage H, 2.24 g of the compound obtained in Stage B of Example 6 and 1.7 ml of triethanolamine are refluxed in 40 ml of toluene for 24 hours. The reaction mixture is concentrated, taken up in ethyl acetate, washed with water and then extracted with 1 N hydrochloric acid, and the extract is rendered basic with concentrated sodium hydroxide solution and extracted with methylene chloride. The extract is dried to yield ethyl N-{1-[(3,4-methylenedioxybenzocyclobuten-1-yl)-methyl]-piperid-4-yl)-N-methylcarbamate. 23.5 ml of a 2% solution of fumaric acid in ethanol are added to yield the desired salt. The reaction mixture is concentrated washed with water extracted with 1 N hydrochloric acid extracted with methylene chloride The extract is dried

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

実験手順: 49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound. are hydrogenated at 50° C. under 5 Kg The catalyst is filtered off the filtrate is evaporated recovered with diethyl ether The ethereal phase is dried evaporated