[1-(环丙基甲基)吡咯烷-2-基]甲胺

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5.8 g of 2-methoxy-5-sulphamoyl benzoic acid, 50 ml of acetone, 10 ml of water and 3.6 ml of triethylamine (density 0.726) are placed in a 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The solution is cooled to about +10° C., then 3.6 g of isobutyl chloroformate is added drop by drop. The medium is reacted for 30 minutes at 0° C., after which 4.5 g of 1-cyclopropylmethyl-2-aminomethyl-pyrrolidine is poured in drop by drop. The medium is reacted for 1 hour at room temperature, 50 ml of water is added and the acetone is evaporated under vacuum. The reaction medium is further diluted with 50 ml of water and made alkaline with 10 ml of ammonia (density 0.91). The viscous product which is precipitated crystallises slowly. The solid is filtered off, washed with water and re-crystallised in 50 ml of ethanol. 3.8 g 841%) of benzamide is obtained, melting at 177° C. fitted with an agitator The solution is cooled to about +10° C. The medium is reacted for 30 minutes at 0° C. The medium is reacted for 1 hour at room temperature the acetone is evaporated under vacuum The reaction medium is further diluted with 50 ml of water The viscous product which is precipitated crystallises slowly The solid is filtered off washed with water re-crystallised in 50 ml of ethanol

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 4.3 g of 1-cyclopropylmethyl-2-aminomethylpyrrolidine (0.028 mole) and 40 ml of methylethyl ketone are placed in 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The mixture is cooled to about 10° C. and a solution of 7.6 g of 2-methoxy-3-isopropyl-5-sulphamoyl-6-methyl benzoyl chloride (0.025 mole) in 50 ml of methyl-ethyl-ketone is poured in drop by drop. The mixture is reacted for 1 hour at room temperature then evaporated dry under vacuum, and the residue is dissolved in 100 ml of water and 10 ml of hydrochloric acid (density 1.18). The solution is sucked up under vacuum to eliminate the last traces of solvent, an insoluble component is filtered off and the filtrate is made alkaline with 15 ml of ammonia (density=0.91). The precipitate formed is filtered, washed with water and re-crystallised moist in 50 ml of ethyl acetate. 2.5 g (24%) of product is obtained, melting at about 125° C. fitted with an agitator The mixture is reacted for 1 hour at room temperature then evaporated dry under vacuum the residue is dissolved in 100 ml of water an insoluble component is filtered off The precipitate formed is filtered washed with water re-crystallised moist in 50 ml of ethyl acetate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5.8 g of 2-methoxy-5-sulphamoyl benzoic acid, 50 ml of acetone, 10 ml of water and 3.6 ml of triethylamine (density 0.726) are placed in a 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The solution is cooled to about +10° C., then 3.6 g of isobutyl chloroformate is added drop by drop. The medium is reacted for 30 minutes at 0° C., after which 4.5 g of 1-cyclopropylmethyl-2-aminomethyl-pyrrolidine is poured in drop by drop. The medium is reacted for 1 hour at room temperature, 50 ml of water is added and the acetone is evaporated under vacuum. The reaction medium is further diluted with 50 ml of water and made alkaline with 10 ml of ammonia (density 0.91). The viscous product which is precipitated crystallises slowly. The solid is filtered off, washed with water and re-crystallised in 50 ml of ethanol. 3.8 g 841%) of benzamide is obtained, melting at 177° C. fitted with an agitator The solution is cooled to about +10° C. The medium is reacted for 30 minutes at 0° C. The medium is reacted for 1 hour at room temperature the acetone is evaporated under vacuum The reaction medium is further diluted with 50 ml of water The viscous product which is precipitated crystallises slowly The solid is filtered off washed with water re-crystallised in 50 ml of ethanol

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 4.3 g of 1-cyclopropylmethyl-2-aminomethylpyrrolidine (0.028 mole) and 40 ml of methylethyl ketone are placed in 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The mixture is cooled to about 10° C. and a solution of 7.6 g of 2-methoxy-3-isopropyl-5-sulphamoyl-6-methyl benzoyl chloride (0.025 mole) in 50 ml of methyl-ethyl-ketone is poured in drop by drop. The mixture is reacted for 1 hour at room temperature then evaporated dry under vacuum, and the residue is dissolved in 100 ml of water and 10 ml of hydrochloric acid (density 1.18). The solution is sucked up under vacuum to eliminate the last traces of solvent, an insoluble component is filtered off and the filtrate is made alkaline with 15 ml of ammonia (density=0.91). The precipitate formed is filtered, washed with water and re-crystallised moist in 50 ml of ethyl acetate. 2.5 g (24%) of product is obtained, melting at about 125° C. fitted with an agitator The mixture is reacted for 1 hour at room temperature then evaporated dry under vacuum the residue is dissolved in 100 ml of water an insoluble component is filtered off The precipitate formed is filtered washed with water re-crystallised moist in 50 ml of ethyl acetate