Реакция #63345
ord-c5fa03e0c1ec46999ab8fa5c993f6693
Уравнение реакции
carbon disulphide
3-(1-piperidinylmethyl)phenoxy propanamine
Triethylamine
→
title compound
[3-[3-(1-Piperidinylmethyl)phenoxy]propyl]isothiocyanate
Реагенты
Условия реакции
Температура
-14°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураthe mixture was heated
- 2Температураat reflux for 45 minutes
- 3ФильтрацияThe resulting suspension was purified by filtration
- 4Другоеthe filtrate evaporated in vacuo
- 5ДругоеThe residue was purified by column chromatography
Методика
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.