반응 #63345

반응 방정식

carbon disulphide

3-(1-piperidinylmethyl)phenoxy propanamine

Triethylamine

→

title compound

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

용매

acetone

acetone

acetone

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도at reflux for 45 minutes
3. 3
   여과The resulting suspension was purified by filtration
4. 4
   기타the filtrate evaporated in vacuo
5. 5
   기타The residue was purified by column chromatography

실험 절차

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.

출처