Hydrochloric Acid → HCID 178526659, compound

Participants

Reaction Steps

A solution of 1.65 mL (0.02 mol) of 1,3-diaminopropane in toluene (10 mL) was cooled to -10° C. using an ice/methanol bath. To this solution was added 2,6-dichloro-4-nitrophenylisothiocyanate (2.45 g, 0.01 mol) in toluene (10 mL) dropwise over 30 minutes, which reacted to form a red oil. The reaction was stirred for an additional 2 hours, then heated at reflux for 4 hours. The mixture was cooled to room temperature then treated with 30 mL of 1 M HCl. After filtration of some insoluble material, the biphasic mixture was separated and the aqueous phase was basified to pH 9 using 1M NaOH. The resulting yellow precipitate was collected by filtration, washed with water, then hexane and air dried to give 0.6 g (21%) of the product.

Provenance & Evidence