反应详情

25 ml of methanol, 40 ml of acetone and 0.1 ml of concentrated hydrochloric acid were added to 1.8 g (4.4 mmol) of N1-(3′,4′-dichlorobenzyl)-N5-octyl-biguanide hydrochloride, and the mixture was refluxed for 24 hours. The solvent was distilled of f under reduced pressure, and the residue was dissolved in 80% aqueous acetonitrile. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 0.5 g of a colorless resinous solid (1) from the first main elution fraction with a mixture of chloroform and methanol (95:5), and 0.7 g of a colorless resinous solid (2) from the second main elution fraction.

1. temperaturethe mixture was refluxed for 24 hours
2. distillationThe solvent was distilled of f under reduced pressure
3. dissolutionthe residue was dissolved in 80% aqueous acetonitrile
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography