N-(2-羟基丙基)乙二胺

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

实验步骤: A 100 g portion of (N-2-hydroxypropyl)ethylenediamine was dissolved in 500 ml of ethanol, then cooled to -10° C. and 55 ml of carbon disulfide was added. Another 500 ml of ethanol was added, the mixture was stirred 30 minutes and then the precipitate was collected, washed with ether and dried. This solid was heated at 140°-150° C. until hydrogen sulfide evolution ceased and then cooled to room temperature. The solid was dissolved in 500 ml of boiling water, treated with charcoal, clarified and cooled at 4° C. overnight. The solid was collected, washed with water and dried at 60° C. in vacuo, giving 34.1 g of 1-(2-hydroxypropyl)-2-imidazolidinethione mp 101°-102° C. the precipitate was collected washed with ether dried This solid was heated at 140°-150° C. until hydrogen sulfide evolution cooled to room temperature The solid was dissolved in 500 ml of boiling water treated with charcoal cooled at 4° C. overnight The solid was collected washed with water dried at 60° C. in vacuo

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

实验步骤: A 100 g portion of (N-2-hydroxypropyl)ethylenediamine was dissolved in 500 ml of ethanol, then cooled to -10° C. and 55 ml of carbon disulfide was added. Another 500 ml of ethanol was added, the mixture was stirred 30 minutes and then the precipitate was collected, washed with ether and dried. This solid was heated at 140°-150° C. until hydrogen sulfide evolution ceased and then cooled to room temperature. The solid was dissolved in 500 ml of boiling water, treated with charcoal, clarified and cooled at 4° C. overnight. The solid was collected, washed with water and dried at 60° C. in vacuo, giving 34.1 g of 1-(2-hydroxypropyl)-2-imidazolidinethione mp 101°-102° C. the precipitate was collected washed with ether dried This solid was heated at 140°-150° C. until hydrogen sulfide evolution cooled to room temperature The solid was dissolved in 500 ml of boiling water treated with charcoal cooled at 4° C. overnight The solid was collected washed with water dried at 60° C. in vacuo

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

实验步骤: Synthesis was performed from (2S)-2-({(2S)-2-[(tert-butoxycarbonyl)amino]-3-phenylpropanoyl}amino)-3-[3-(methoxycarbonyl)-4-(2-methoxy-2-oxoethoxy)phenyl]propanoic acid and N-(2-hydroxypropyl)ethylenediamine (34 mg) according to Method B to give the title compound (26 mg). 1H-NMR (400 MHz, CD3OD) d 7.56 (d, J=2.4 Hz, 1H), 7.32 (d, J=8.8 Hz, 1H), 7.28-7.17 (m, 5H), 7.05 (d, J=8.5 Hz, 1H), 4.37 (m, 1H), 4.27 (dd, J=5.2 Hz, J=8.9 Hz, 1H), 1.35 (s, 9H), 1.22 (dd, J=1.8 Hz, J=6.3 Hz, 3H); HRMS m/z 630.2883 (calc. of monoisotopic mass for C31H42N4O10 gives 630.2901). Synthesis

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

实验步骤: A 100 g portion of (N-2-hydroxypropyl)ethylenediamine was dissolved in 500 ml of ethanol, then cooled to -10° C. and 55 ml of carbon disulfide was added. Another 500 ml of ethanol was added, the mixture was stirred 30 minutes and then the precipitate was collected, washed with ether and dried. This solid was heated at 140°-150° C. until hydrogen sulfide evolution ceased and then cooled to room temperature. The solid was dissolved in 500 ml of boiling water, treated with charcoal, clarified and cooled at 4° C. overnight. The solid was collected, washed with water and dried at 60° C. in vacuo, giving 34.1 g of 1-(2-hydroxypropyl)-2-imidazolidinethione mp 101°-102° C. the precipitate was collected washed with ether dried This solid was heated at 140°-150° C. until hydrogen sulfide evolution cooled to room temperature The solid was dissolved in 500 ml of boiling water treated with charcoal cooled at 4° C. overnight The solid was collected washed with water dried at 60° C. in vacuo