Hydrochloric Acid → HCID 22640009, compound

Participants

Reaction Steps

112 g (0.286 mol) of (4-benzyloxybenzyl)(5-Chloro-2,6-dimethylpyrimidin-4-yl)amine hydrochloride (from example A1) are suspended in ethanol (1.1 l) and 12.5 N hydrochloric acid (1.1 l) and the suspension is heated at reflux for 1 h. The yellow solution is cooled to room temperature and stirred into ice-water (4 l). The solution is then adjusted to a pH of 8 using 10 N sodium hydroxide solution and extracted with ethyl acetate (3×1 l). The combined organic extracts are washed with water (1 l), dried over sodium sulfate and concentrated to a volume of about 100 ml. The residue is taken up in ethyl acetate (100 ml) and diisopropyl ether (200 ml) and stirred at room temperature for 15 min. The crystals are filtered and washed with diisopropyl ether/ethyl acetate) (2:1). Drying in a vacuum drying cabinet at 40° C. gives 38.4 g (51%) of the title compound as a pale beige solid. m.p.: 202° C.

Provenance & Evidence