N-ethylcycloheptanamine

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: N-ethylcycloheptylamine (21.15 g) was added with ice bath cooling to a mixture consisting of trichloromethylchloroformate (29.7 g) end ethyl acetate (300 ml). Thereafter, the temperature was gradually elevated and heated with refluxing for 6 hours. After distilling off the solvent, the obtained oil was distilled under reduced pressure to obtain N-cycloheptyl -N-ethylcarbamoyl chloride (17.20 g). b.p. 125°-128° C./4.0 mbar. cooling to a mixture heated with refluxing for 6 hours After distilling off the solvent the obtained oil was distilled under reduced pressure

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

実験手順: N-ethylcycloheptylamine (21.15 g) was added with ice bath cooling to a mixture consisting of trichloromethylchloroformate (29.7 g) end ethyl acetate (300 ml). Thereafter, the temperature was gradually elevated and heated with refluxing for 6 hours. After distilling off the solvent, the obtained oil was distilled under reduced pressure to obtain N-cycloheptyl -N-ethylcarbamoyl chloride (17.20 g). b.p. 125°-128° C./4.0 mbar. cooling to a mixture heated with refluxing for 6 hours After distilling off the solvent the obtained oil was distilled under reduced pressure

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium borohydride (3.78 g) was gradually added with ice bath cooling to a methanol (600 ml) solution of N-ethylidenecycloheptylamine (41.7 g) and agitated at 10° C. for 3 hours. Thereafter, the solvent was distilled off, followed by extraction with methylene chloride. Then, the extract was dried over anhydrous magnesium sulfate. Methylene chloride was distilled off and the obtained oil was distilled under reduced pressure to obtain N-ethylcycloheptylamine (35.96 g). b.p. 110°-113° C./26.6 mbar. Thereafter, the solvent was distilled off followed by extraction with methylene chloride Then, the extract was dried over anhydrous magnesium sulfate Methylene chloride was distilled off the obtained oil was distilled under reduced pressure

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium borohydride (3.78 g) was gradually added with ice bath cooling to a methanol (600 ml) solution of N-ethylidenecycloheptylamine (41.7 g) and agitated at 10° C. for 3 hours. Thereafter, the solvent was distilled off, followed by extraction with methylene chloride. Then, the extract was dried over anhydrous magnesium sulfate. Methylene chloride was distilled off and the obtained oil was distilled under reduced pressure to obtain N-ethylcycloheptylamine (35.96 g). b.p. 110°-113° C./26.6 mbar. Thereafter, the solvent was distilled off followed by extraction with methylene chloride Then, the extract was dried over anhydrous magnesium sulfate Methylene chloride was distilled off the obtained oil was distilled under reduced pressure

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

実験手順: N-ethylcycloheptylamine (21.15 g) was added with ice bath cooling to a mixture consisting of trichloromethylchloroformate (29.7 g) end ethyl acetate (300 ml). Thereafter, the temperature was gradually elevated and heated with refluxing for 6 hours. After distilling off the solvent, the obtained oil was distilled under reduced pressure to obtain N-cycloheptyl -N-ethylcarbamoyl chloride (17.20 g). b.p. 125°-128° C./4.0 mbar. cooling to a mixture heated with refluxing for 6 hours After distilling off the solvent the obtained oil was distilled under reduced pressure

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium borohydride (3.78 g) was gradually added with ice bath cooling to a methanol (600 ml) solution of N-ethylidenecycloheptylamine (41.7 g) and agitated at 10° C. for 3 hours. Thereafter, the solvent was distilled off, followed by extraction with methylene chloride. Then, the extract was dried over anhydrous magnesium sulfate. Methylene chloride was distilled off and the obtained oil was distilled under reduced pressure to obtain N-ethylcycloheptylamine (35.96 g). b.p. 110°-113° C./26.6 mbar. Thereafter, the solvent was distilled off followed by extraction with methylene chloride Then, the extract was dried over anhydrous magnesium sulfate Methylene chloride was distilled off the obtained oil was distilled under reduced pressure

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: N-ethylcycloheptylamine (21.15 g) was added with ice bath cooling to a mixture consisting of trichloromethylchloroformate (29.7 g) end ethyl acetate (300 ml). Thereafter, the temperature was gradually elevated and heated with refluxing for 6 hours. After distilling off the solvent, the obtained oil was distilled under reduced pressure to obtain N-cycloheptyl -N-ethylcarbamoyl chloride (17.20 g). b.p. 125°-128° C./4.0 mbar. cooling to a mixture heated with refluxing for 6 hours After distilling off the solvent the obtained oil was distilled under reduced pressure

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Sodium borohydride (3.78 g) was gradually added with ice bath cooling to a methanol (600 ml) solution of N-ethylidenecycloheptylamine (41.7 g) and agitated at 10° C. for 3 hours. Thereafter, the solvent was distilled off, followed by extraction with methylene chloride. Then, the extract was dried over anhydrous magnesium sulfate. Methylene chloride was distilled off and the obtained oil was distilled under reduced pressure to obtain N-ethylcycloheptylamine (35.96 g). b.p. 110°-113° C./26.6 mbar. Thereafter, the solvent was distilled off followed by extraction with methylene chloride Then, the extract was dried over anhydrous magnesium sulfate Methylene chloride was distilled off the obtained oil was distilled under reduced pressure