2-苯基丙烷-1,2-二胺

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

实验步骤: 2-Amino-6-chloro-4-hydroxy-5-nitropyrimidine (0.626 g; 3.0 mmole) was dissolved in 130 ml of refluxing absolute ethanol and 0.45 g of 1,2-diamino-2-phenylpropane free-base (3.0 mmole) was added all at once dissolved in 8 ml of absolute ethanol. The mixture was stirred and maintained at reflux as a light yellow precipitate formed. Analysis by HPLC at 30 minutes showed a marked slowing of the condensation after a little over one-half of the reactants had been consumed. (Partisil SCX column (25×0.46 cm) eluted with 0.1M ammonium hydroxide made to pH 3.3 with formic acid/methanol, 3:2 v/v). Completion of the reaction to within 97% utilization of the diamine was accomplished by addition of 3.6 ml of 1M triethylamine in absolute ethanol (3.6 mmole) followed by 0.063 g of the above pyrimidine, the reaction being refluxed an additional hour. After being kept overnight at -15° C. the majority of the somewhat gelatinous product was collected by centrifugation, washed with 10 ml cold ethanol, and finally, twice with 30 ml each of ethyl ether. A second crop of equal purity was collected after allowing the mother liquor supernate to stand for an additional 5 days at -15° C., and similarly washed. These materials dried under vacuum in the presence of P2O5 gave 0.97 g (0.889+0.081) of the monohydrochloride salt for a yield of 95% based upon diamine. was added maintained at reflux as a light yellow precipitate formed a marked slowing of the condensation after a little over one-half of the reactants had been consumed (Partisil SCX column (25×0.46 cm) eluted with 0.1M ammonium hydroxide made to pH 3.3 with formic acid/methanol, 3:2 v/v) Completion of the reaction to within 97% utilization of the diamine the reaction being refluxed an additional hour After being kept overnight at -15° C. the majority of the somewhat gelatinous product was collected by centrifugation washed with 10 ml cold ethanol A second crop of equal purity was collected to stand for an additional 5 days at -15° C. similarly washed These materials dried under vacuum in the presence of P2O5

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

实验步骤: 2-Amino-6-chloro-4-hydroxy-5-nitropyrimidine (0.626 g; 3.0 mmole) was dissolved in 130 ml of refluxing absolute ethanol and 0.45 g of 1,2-diamino-2-phenylpropane free-base (3.0 mmole) was added all at once dissolved in 8 ml of absolute ethanol. The mixture was stirred and maintained at reflux as a light yellow precipitate formed. Analysis by HPLC at 30 minutes showed a marked slowing of the condensation after a little over one-half of the reactants had been consumed. (Partisil SCX column (25×0.46 cm) eluted with 0.1M ammonium hydroxide made to pH 3.3 with formic acid/methanol, 3:2 v/v). Completion of the reaction to within 97% utilization of the diamine was accomplished by addition of 3.6 ml of 1M triethylamine in absolute ethanol (3.6 mmole) followed by 0.063 g of the above pyrimidine, the reaction being refluxed an additional hour. After being kept overnight at -15 ° C. the majority of the somewhat gelatinous product was collected by centrifugation, washed with 10 ml cold ethanol, and finally, twice with 30 ml each of ethyl ether. A second crop of equal purity was collected after allowing the mother liquor supernate to stand for an additional 5 days at -15° C., and similarly washed. These materials dried under vacuum in the presence of P2O5 gave 0.97 g (0.889+0.081) of the monohydrochloride salt for a yield of 95% based upon diamine. was added maintained at reflux as a light yellow precipitate formed a marked slowing of the condensation after a little over one-half of the reactants had been consumed (Partisil SCX column (25×0.46 cm) eluted with 0.1M ammonium hydroxide made to pH 3.3 with formic acid/methanol, 3:2 v/v) Completion of the reaction to within 97% utilization of the diamine the reaction being refluxed an additional hour After being kept overnight at -15 ° C. the majority of the somewhat gelatinous product was collected by centrifugation washed with 10 ml cold ethanol A second crop of equal purity was collected to stand for an additional 5 days at -15° C. similarly washed These materials dried under vacuum in the presence of P2O5