Hydrochloric Acid → HCID 21094303, compound

Participants

Reaction Conditions

Reaction Steps

Formic acid (0.55 ml) and 37% formaldehyde (0.6 ml) are added at 0° C. to the compound obtained in Example 4 (1.8 g; 7.2 mmol) in the form of a base. The reaction mixture is heated at 80° C. for 24 hours with stirring. After having cooled the reaction mixture to 0° C., 10 ml of 6N HCl are added. The mixture is then washed with ether, rendered alkaline with 2N NaOH and extracted with ether. The organic phase is dried over magnesium sulphate, filtered and evaporated under reduced pressure. The yellow oil so obtained is purified by chromatography on silica gel (eluant: dichloromethane with the progressive addition of methanol until the proportions 9/1 are reached). The purified oil is taken up in ether saturated with HCl(g) and stirred until a precipitate is obtained, which precipitate is then suction-filtered off and placed under a vacuum in a dessicator to yield the title product in the form of a very hygroscopic white solid.

Provenance & Evidence