Reaktion #63345

Reaktionsgleichung

carbon disulphide

3-(1-piperidinylmethyl)phenoxy propanamine

Triethylamine

→

title compound

[3-[3-(1-Piperidinylmethyl)phenoxy]propyl]isothiocyanate

Lösungsmittel

acetone

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturat reflux for 45 minutes
3. 3
   FiltrationThe resulting suspension was purified by filtration
4. 4
   Sonstigethe filtrate evaporated in vacuo
5. 5
   SonstigeThe residue was purified by column chromatography

Vorschrift

A solution of carbon disulphide (3.3 ml) in acetone (8 ml) was added dropwise to a solution of 3-[3-(1-piperidinylmethyl)phenoxy propanamine (12.4 g) in acetone (30 ml) over a 15 minute period, between -5° and -10° C. The solution was cooled to -14° C. and mercury (II) chloride (13.6 g) in acetone (30 ml) was added, during 45 minutes. Triethylamine (16 ml) was added at 0° C. during 15 minutes, and the mixture was heated at reflux for 45 minutes. The resulting suspension was purified by filtration and the filtrate evaporated in vacuo. The residue was purified by column chromatography using methanol as eluant to give the title compound (6 g) as an amber oil.

Quelle