Hydrochloric Acid → HCID 20564657, compound

Participants

Reaction Steps

106 g (1 mole) of 1-hydroxy-3-thiapentane were boiled under reflux for 3 hours with 76 g (1 mole) of thiourea and 110 g (1.1 mole) of 37% hydrochloric acid. A solution of 68 g (1.21 moles) of potassium hydroxide in 100 ml of water was then added dropwise with stirring at 313° to 323° K. After heating for 40 minutes to 363° K., the 3-thiapentane-1-thiol precipitated was separated off in a separation funnel and dissolved under nitrogen at 303° to 313° K. in 400 g of 40% KOH (2.85 moles of KOH) accommodated in a 1000 ml three-necked flask. A solution of 130 g of 3-chloropropylamine hydrochloride (1 mole) in 160 ml of water was then added dropwise with stirring at 343° K. After stirring for another 3 hours at 363° K., the mixture was cooled to 323° K. and separated in a separation funnel. The oil phase was fractionated in vacuo twice.

Provenance & Evidence