反応 #4857

反応方程式

HPPh2

LiPPh2

1,3-dichloropropane

n-butyl lithium

→

Ph2P(CH2)3Cl

溶媒

diethyl ether

water

tetrahydrofuran

反応条件

後処理

1. 1
   温度this was slowly warmed to room temperature
2. 2
   その他The 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
   その他The organic layer was separated
6. 6
   その他the solvent removed by vacuum

実験手順

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.

出典