N-benzyl-2,2-difluoroethanamine

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:

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: An amount of 757.9 g (7.39 mol) of 2,2-difluoro-1-chloroethane and 800 g of benzylamine (7.39 mol) are heated in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 1400 g of water are added and the aqueous phase is separated. The organic phase is distilled at standard pressure and the excess 2,2-difluoro-1-chlorethan is distilled off Remaining traces of 2,2-difluoro-1-chloroethane are distilled off under vacuum (200 mbar). An amount of 587 g of N-benzyl-2,2-difluoroethanamine is obtained as residue with a purity of 97.4%. This corresponds to a yield of 93.4%, based on reacted benzylamine. The benzylamine hydrochloride in the aqueous phase can be rereleased by addition of sodium hydroxide solution and be used once again. A further 21 g of N-benzyl-2,2-difluoroethanamine are present in the aqueous phase so that the yield is increased to 96%. the aqueous phase is separated The organic phase is distilled at standard pressure the excess 2,2-difluoro-1-chlorethan is distilled off are distilled off under vacuum (200 mbar)

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

実験手順: An amount of 768.1 g (7.39 mol) of 2,2-difluoro-1-chloroethane and 400 g of benzylamine (3.695 mol) are heated in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 700 g of water are added and the aqueous phase is separated. The organic phase is distilled at standard pressure and the excess 2,2-difluoro-1-chloroethane is distilled off. Remaining traces of 2,2-difluoro-1-chloroethane are distilled off under vacuum (200 mbar). An amount of 304 g of N-benzyl-2,2-difluoroethanamine is obtained as residue with a purity of 97.2%. This corresponds to a yield of 93.4%, based on reacted benzylamine. The benzylamine hydrochloride in the aqueous phase can be rereleased by addition of sodium hydroxide solution and be used once again. the aqueous phase is separated The organic phase is distilled at standard pressure the excess 2,2-difluoro-1-chloroethane is distilled off are distilled off under vacuum (200 mbar)

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

実験手順: An amount of 10 g (92 mmol) of 2,2-difluoro-1-chloroethane, 5 g (46 mmol) of benzylamine and 5.2 g (51 mmol) of triethylamine are heated in 20 g of water in an autoclave at an internal temperature of 120° C. for 6 hours. The two-phase solution is twice extracted with 50 ml of dichloromethane each time and the combined organic phases are washed with 50 ml of water and subsequently distilled. An amount of 5.2 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 66%, based on benzylamine. The two-phase solution is twice extracted with 50 ml of dichloromethane each time the combined organic phases are washed with 50 ml of water subsequently distilled

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

実験手順: An amount of 10 g (92 mmol) of 2,2-difluoro-1-chloroethane, 5 g (46 mmol) of benzylamine, 1 g of potassium bromide and 5.2 g (51 mmol) of triethylamine are heated in 20.6 g of N-methylpyrrolidone in an autoclave at an internal temperature of 120° C. for 6 hours. Subsequently, 100 g of 1N hydrochloric acid are added and the solvent is removed under vacuum. The residue is taken up in 30 ml of dichloromethane and adjusted to pH 8 with solid sodium hydrogencarbonate. The phases are subsequently separated and the aqueous phase is again extracted with 20 ml of dichloromethane. The organic phase is distilled. An amount of 7.4 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 94%, based on benzylamine. the solvent is removed under vacuum The phases are subsequently separated the aqueous phase is again extracted with 20 ml of dichloromethane The organic phase is distilled

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

実験手順: An amount of 10 g (92 mmol) of 2,2-difluoro-1-chloroethane, 5 g (46 mmol) of benzylamine and 5.2 g (51 mmol) of triethylamine are heated in 20.6 g of N-methylpyrrolidone in an autoclave at an internal temperature of 120° C. for 6 hours. Subsequently, 100 g of 1N hydrochloric acid are added and the solvent is removed under vacuum. The residue is taken up in 30 ml of dichloromethane and adjusted to pH 8 with solid sodium hydrogencarbonate. The phases are subsequently separated and the aqueous phase is again extracted with 20 ml of dichloromethane. The organic phase is distilled. An amount of 7.3 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 93%, based on benzylamine. the solvent is removed under vacuum The phases are subsequently separated the aqueous phase is again extracted with 20 ml of dichloromethane The organic phase is distilled

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

実験手順: An amount of 10 g (92 mmol) of 2,2-difluoro-1-chloroethane, 5 g (46 mmol) of benzylamine and 5.2 g (51 mmol) of triethylamine are heated in 18.7 g of N,N-dimethylacetamide in an autoclave at an internal temperature of 120° C. for 6 hours. Subsequently, 100 g of 1N hydrochloric acid are added and the solvent is removed under vacuum. The residue is taken up in 30 ml of dichloromethane and adjusted to pH 8 with solid sodium hydrogencarbonate. The phases are subsequently separated and the aqueous phase is again extracted with 20 ml of dichloromethane. The organic phase is distilled. An amount of 7.1 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 90%, based on benzylamine the solvent is removed under vacuum The phases are subsequently separated the aqueous phase is again extracted with 20 ml of dichloromethane The organic phase is distilled

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

実験手順: An amount of 5 g (49.7 mmol) of 2,2-difluoro-1-chloroethane and 11.3 g (105 mmol) of benzylamine are heated in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 100 g of 1N hydrochloric acid are added and the solvent is removed under vacuum. The residue is taken up in 50 ml of water and 50 ml of dichloromethane and adjusted to pH 8 with solid sodium hydrogencarbonate. The phases are subsequently separated and the aqueous phase is again extracted with 20 ml of dichloromethane. The organic phase is distilled. An amount of 3.5 g of N-benzyl-2,2-difluoroethanamine is obtained, which corresponds to a yield of 41%, based on 2,2-difluoro-1-chloroethane used. the solvent is removed under vacuum The phases are subsequently separated the aqueous phase is again extracted with 20 ml of dichloromethane The organic phase is distilled