Water → HCID 131722239, compound

Participants

Reaction Steps

To a solution of (3-(5-bromo(3-pyridyloxy))propyl)methylamine (0.790 g, 3.22 mmol) in ethanol (12 mL) was added galactaric acid (339.0 mg, 1.61 mmol). Water (3.4 mL) was added dropwise, while warming the light-yellow solution to near reflux. To remove some white, insoluble crystals, the warm solution was filtered through a glass wool plug, washing the filter plug with a warm solution of ethanol-water (4:1, v/v) (3.8 mL). The filtrate was diluted with ethanol (18 mL), producing a light-beige precipitate. The mixture was allowed to cool to ambient temperature and was further cooled at 5° C. for 48 h. The precipitate was filtered, washed with ethanol (5 mL), vacuum dried at 40° C. for 24 h to give 983.3 mg (68.8%) of a glassy, beige powder, mp 166-173.5° C.

Provenance & Evidence