Hydrochloric Acid → HCID 131725035, compound

Participants

Reaction Steps

(2,4-Dinitro-phenyl)-dipropyl-amine (13.1 g, 49 mmol) was dissolved in 200 ml ethanol and cooled in an icebath. In succession, ION HCl (60 ml, 600 mmol) and tin(II)chloride (112.5, 499 mmol), were added. The solution was stirred at room temperature 16 h. The reaction mixture was poured into a separatory funnel containing 100 ml ice-cold water followed by the addition of 20% KOH (ice-cold, 1L). The mixture was extracted with ether (3×150 ml). The combined organic phases were washed with water (3×100 ml) and brine, dried with solid MgSO4 and concentrated. Distillation (Krugel Rohr, 90°-100° C. at 0.2 mm Hg) followed by treatment with decolorizing charcoal and recrystallization from 15% ethyl acetate in hexane gave 8.0 g product >99% pure by HPLC.

Provenance & Evidence