反应详情

温度

40 °C

0.20 g (0.85 mmol) N-cyano-N′-(2,6-dimethoxybenzyl)guanidine were suspended in 20 ml methanol/water (1:1). Subsequently, 63.3 mg (0.85 mmol) hydroxyacetone were added and the mixture was heated to 40° C. The pH-value was adjusted at high temperature with 1 N HCl to 2.5-3 pH. In total, the reaction mixture was heated for 34 hours at 40° C. under constant pH-control until no further educts could be detected by mass spectrometry. The methanol was distilled off under vacuum and a white solid remained which was purified by HPLC (Merck: Chromolith RP-18E, 100-25; eluent water/acetonitrile/0.1 molar acetic acid); 64 mg.

1. temperatureIn total, the reaction mixture was heated for 34 hours at 40° C. under constant pH-control until no further educts
2. distillationThe methanol was distilled off under vacuum
3. customwas purified by HPLC (Merck: Chromolith RP-18E, 100-25; eluent water/acetonitrile/0.1 molar acetic acid)