N-(3-氨基丙基)-N-乙基苯胺

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of thiophosgene (7.43 ml) in CH2Cl2 (300 ml) was added dropwise over 11/2 hours at 20° C. under a nitrogen atmosphere to a stirred solution of N-ethyl-N-(3-aminopropyl)aniline (17.8 g) and triethylamine (27.8 ml) in CH2Cl2 (500 ml). The mixture was stirred at 20° C. for a further 1/2 hours then heated under reflux for 11/2 hours. The mixture was allowed to cool, washed with water, dried over MgSO4, filtered and solvent removed from the filtrate in vacuo. The product was purified by chromatography on silica gel eluting with CH2Cl2 to give N-ethyl-N-(3-isothiocyanatopropyl)aniline (7.2 g) as a red oil. then heated under reflux for 11/2 hours to cool washed with water dried over MgSO4 filtered solvent removed from the filtrate in vacuo The product was purified by chromatography on silica gel eluting with CH2Cl2

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of thiophosgene (7.43 ml) in CH2Cl2 (300 ml) was added dropwise over 11/2 hours at 20° C. under a nitrogen atmosphere to a stirred solution of N-ethyl-N-(3-aminopropyl)aniline (17.8 g) and triethylamine (27.8 ml) in CH2Cl2 (500 ml). The mixture was stirred at 20° C. for a further 1/2 hours then heated under reflux for 11/2 hours. The mixture was allowed to cool, washed with water, dried over MgSO4, filtered and solvent removed from the filtrate in vacuo. The product was purified by chromatography on silica gel eluting with CH2Cl2 to give N-ethyl-N-(3-isothiocyanatopropyl)aniline (7.2 g) as a red oil. then heated under reflux for 11/2 hours to cool washed with water dried over MgSO4 filtered solvent removed from the filtrate in vacuo The product was purified by chromatography on silica gel eluting with CH2Cl2

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of thiophosgene (7.43 ml) in CH2Cl2 (300 ml) was added dropwise over 11/2 hours at 20° C. under a nitrogen atmosphere to a stirred solution of N-ethyl-N-(3-aminopropyl)aniline (17.8 g) and triethylamine (27.8 ml) in CH2Cl2 (500 ml). The mixture was stirred at 20° C. for a further 11/2 hours then heated under reflux for 11/2 hours. The mixture was allowed m cool washed with water, dried over MgSO4, filtered and solvent removed from the filtrate in vacuo. The product was purified by chromatography on silica gel eluting with CH2Cl2 to give N-ethyl-N-(3-isothiocyanatopropyl)aniline (72 g) as a red oil. then heated under reflux for 11/2 hours cool washed with water dried over MgSO4 filtered solvent removed from the filtrate in vacuo The product was purified by chromatography on silica gel eluting with CH2Cl2