tert-butyl N-ethyl-N-(3-hydroxypropyl)carbamate

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

实验步骤: 11 g (0.0618 mol) of N-bromosuccinimide are added in the course of 5 minutes, with stirring, to a solution, which has been cooled to 0° C., of 10.49 g (0.0516 mol) of 3-(N-BOC-ethylamino)-1-propanol and 16.23 g (0.0619 mol) of triphenylphosphine in 160 ml of methylene chloride. The reaction mixture is stirred for a further 30 minutes at 0°-20° C. and is then concentrated by evaporation in vacuo. The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms. After filtration and concentration of the filtrate by evaporation in vacuo, the title compound is obtained in the form of an oil, Rf value=0.71 (silica gel/tert-butyl methyl ether). The reaction mixture is stirred for a further 30 minutes at 0°-20° C. is then concentrated by evaporation in vacuo The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms After filtration and concentration of the filtrate by evaporation in vacuo

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

实验步骤: 11 g (0.0618 mol) of N-bromosuccinimide are added in the course of 5 minutes, with stirring, to a solution, which has been cooled to 0° C., of 10.49 g (0.0516 mol) of 3-(N-BOC-ethylamino)-1-propanol and 16.23 g (0.0619 mol) of triphenylphosphine in 160 ml of methylene chloride. The reaction mixture is stirred for a further 30 minutes at 0°-20° C. and is then concentrated by evaporation in vacuo. The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms. After filtration and concentration of the filtrate by evaporation in vacuo, the title compound is obtained in the form of an oil, Rf value=0.71 (silica gel/tert-butyl methyl ether). The reaction mixture is stirred for a further 30 minutes at 0°-20° C. is then concentrated by evaporation in vacuo The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms After filtration and concentration of the filtrate by evaporation in vacuo

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

实验步骤: 11 g (0.0618 mol) of N-bromosuccinimide are added in the course of 5 minutes, with stirring, to a solution, which has been cooled to 0° C., of 10.49 g (0.0516 mol) of 3-(N-BOC-ethylamino)-1-propanol and 16.23 g (0.0619 mol) of triphenylphosphine in 160 ml of methylene chloride. The reaction mixture is stirred for a further 30 minutes at 0°-20° C. and is then concentrated by evaporation in vacuo. The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms. After filtration and concentration of the filtrate by evaporation in vacuo, the title compound is obtained in the form of an oil, Rf value=0.71 (silica gel/tert-butyl methyl ether). The reaction mixture is stirred for a further 30 minutes at 0°-20° C. is then concentrated by evaporation in vacuo The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms After filtration and concentration of the filtrate by evaporation in vacuo

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

实验步骤: 11 g (0.0618 mol) of N-bromosuccinimide are added in the course of 5 minutes, with stirring, to a solution, which has been cooled to 0° C., of 10.49 g (0.0516 mol) of 3-(N-BOC-ethylamino)-1-propanol and 16.23 g (0.0619 mol) of triphenylphosphine in 160 ml of methylene chloride. The reaction mixture is stirred for a further 30 minutes at 0°-20° C. and is then concentrated by evaporation in vacuo. The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms. After filtration and concentration of the filtrate by evaporation in vacuo, the title compound is obtained in the form of an oil, Rf value=0.71 (silica gel/tert-butyl methyl ether). The reaction mixture is stirred for a further 30 minutes at 0°-20° C. is then concentrated by evaporation in vacuo The dark-colored oily residue is stirred with 200 ml of hexane, whereupon a brown precipitate forms After filtration and concentration of the filtrate by evaporation in vacuo