Hydrochloric Acid → 1-Amino-3,6-dithianonane

76.4 g (0.164 mole) of 1-hydroxy-3-thiahexane, produced from propane-1-thiol and 2-chloroethanol in the presence of the equivalent quantity of sodium hydroxide were boiled under reflux for 2 hours with 50 g of thiourea and 77 g of 37% hydrochloric acid. After cooling, 32 g (0.8 mole) of sodium hydroxide in 60 ml of water were added to the clear solution of the isothiuronium salt. Thereafter the mixture was heated for 30 minutes on a steam bath. The 1-mercapto-3-thiahexane precipitated was separated off in a separation funnel and was dissolved under nitrogen in a solution of 68 g (1.7 moles) of sodium hydroxide in 130 ml of water accommodated in a three-necked flask. A total of 74.5 g of 2-chloroethylamine hydrochloride in 200 ml of water was added dropwise to the resulting solution at 333° K. After 1 hour on a steam bath, the amine phase precipitated was separated off with ether (300 ml), dried with 40 g of KOH flakes, concentrated by evaporation and fractionated in vacuo.

1. temperatureAfter cooling
2. temperatureThereafter the mixture was heated for 30 minutes on a steam bath
3. customThe 1-mercapto-3-thiahexane precipitated
4. customwas separated off in a separation funnel
5. customaccommodated in a three-necked flask
6. customthe amine phase precipitated
7. customwas separated off with ether (300 ml)
8. dry with materialdried with 40 g of KOH flakes
9. concentrationconcentrated by evaporation

ORD 기록

ord-1c0d239cadd6416db2e7deb6dc93983e

출처 데이터셋

uspto-grants-1981_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04297439