Reaktion #4857

Reaktionsgleichung

HPPh2

LiPPh2

1,3-dichloropropane

n-butyl lithium

→

Ph2P(CH2)3Cl

Lösungsmittel

diethyl ether

water

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthis was slowly warmed to room temperature
2. 2
   SonstigeThe solution was transferred to a dropping funnel
3. 3
   workup.ADDITIONadded dropwise to a flask
4. 4
   workup.STIRRINGAfter stirring overnight the mixture
5. 5
   SonstigeThe organic layer was separated
6. 6
   Sonstigethe solvent removed by vacuum

Vorschrift

To a 500 mL round bottom flask there was added 400 mL of dry tetrahydrofuran followed by 0.081 mole of HPPh2. The mixture was cooled to 0° C. and 0.081 mole of n-butyl lithium was slowly added to generate LiPPh2 ; this was slowly warmed to room temperature and stirred for about one hour. The solution was transferred to a dropping funnel and added dropwise to a flask containing 100 mL of 1,3-dichloropropane dissolved in 100 mL of diethyl ether. After stirring overnight the mixture was hydrolyzed with 25 mL of water. The organic layer was separated and the solvent removed by vacuum to leave Ph2P(CH2)3Cl that was stored under nitrogen until needed.

Quelle