反应详情

100 ml of ethanol, 8.8 ml (37.1 mmol) of 1-tridecanal and 0.8 ml of concentrated hydrochloric acid were added to 5.0 g (18.4 mmol) of N1-(4-methoxyphenethyl)-biguanide hydrochloride, and the mixture was refluxed for 22 hours. The solvent was distilled of f under reduced pressure, and the residue was purified by silica gel column chromatography. The first main fraction eluted with a mixture of chloroform and methanol (9:1.5) was recrystallized from 70% aqueous acetonitrile to obtain 0.92 g of colorless crystals (1) having a melting point of 100 to 102° C., and the second main eluate was recrystallized from 70% aqueous acetonitrile to obtain 1.1 g of colorless crystals (2) having a melting point of 165 to 170° C.

1. temperaturethe mixture was refluxed for 22 hours
2. distillationThe solvent was distilled of f under reduced pressure
3. customthe residue was purified by silica gel column chromatography
4. washThe first main fraction eluted with a mixture of chloroform and methanol (9:1.5)
5. customwas recrystallized from 70% aqueous acetonitrile