Reaktion #1817257

Reaktionsgleichung

3-(4-bromophenacyl)-2,3,5,6-tetrahydrothiopyran-4-one

2-amino-1-dimethylaminopropane

hydrogen chloride

→

1-(1-dimethylamino-2-propyl)-2-(4-bromophenyl)-1,4,6,7-tetrahydrothiopyrano[4,3-b]pyrrole hydrochloride

Lösungsmittel

ethanol

ethanol

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 3 hours
2. 2
   Filtrationfiltered
3. 3
   Sonstigeto provide a solid product
4. 4
   SonstigeRecrystallization from ethanol

Vorschrift

A solution of 5.5 g (0.017 mole) of 3-(4-bromophenacyl)-2,3,5,6-tetrahydrothiopyran-4-one [Example 2 (a)], 1.6 g of 2-amino-1-dimethylaminopropane, 16 ml. of ethanol, and one drop of concentrated hydrochloric acid is heated under reflux for 3 hours, cooled to 5°C, and filtered to provide a solid product. The resulting product is dissolved in ethanol, the solution is acidified with ethereal hydrogen chloride and diluted to the cloud point with ether. Upon standing, a solid separates. Recrystallization from ethanol gives off-white crystals of 1-(1-dimethylamino-2-propyl)-2-(4-bromophenyl)-1,4,6,7-tetrahydrothiopyrano[4,3-b]pyrrole hydrochloride, m.p. 237° to 238°C. dec.

Quelle