Reaktion #1734739

Reaktionsgleichung

thieno[3,2-b]thiophenyl lithium

octadecyl bromide

ammonium chloride

n-butyllithium

thieno[3,2-b]thiophene

sulfur

→

2-Octadecylthiothieno[3,2-b]thiophene

Lösungsmittel

diethyl ether

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 30 minutes
2. 2
   TemperaturAfter renewed cooling by means of an ice bath
3. 3
   workup.ADDITIONare then added dropwise
4. 4
   workup.STIRRINGAfter the mixture has been stirred overnight at room temperature

Vorschrift

47 ml (75 mmol) of 1.6N n-butyllithium are added dropwise at room temperature under nitrogen as blanketing gas to 10 g (71 mmol) of thieno[3,2-b]thiophene dissolved in dry diethyl ether. The mixture is then allowed to reflux for 30 minutes. Subsequently, 2.4 g (75 mmol) of dried sulfur are added with ice cooling and vigorous stirring to the resulting suspension of the thieno[3,2-b]thiophenyl lithium salt. The mixture is then allowed to warm to room temperature and stirred for 60 minutes. After renewed cooling by means of an ice bath, 23.7 g (71 mmol) of octadecyl bromide dissolved in 100 ml of dry diethyl ether are then added dropwise. After the mixture has been stirred overnight at room temperature, 50 ml of 25% ammonium chloride solution are added with ice cooling.

Quelle