Hydrochloric Acid → HCID 21094273, compound

Participants

Reaction Conditions

Reaction Steps

The formaldehyde obtained in Step C (6.8 g; 23 mmol) is dissolved in 100 ml of acetonitrile, then the reaction mixture is heated to approximately 60° C. Phosphorus oxychloride (7 ml) is added to the solution, which is heated at reflux for 6 hours with stirring and then evaporated under reduced pressure. The residue obtained is taken up twice in ethanol and evaporated under reduced pressure, and is then taken up in water. The aqueous phase is washed with dichloromethane and then rendered alkaline with a saturated sodium hydrogen carbonate solution and extracted with dichloromethane. The organic phase is dried over magnesium sulphate, filtered and evaporated under reduced pressure. The oil obtained is taken un in ether saturated with HCl(g) and then evaporated under reduced pressure. The residue is taken up in toluene in the heated state and is stirred until precipitation occurs. The precipitate obtained is then suction-filtered off and the title product is obtained in the form of a white solid.

Provenance & Evidence