Reaktion #1808641

Reaktionsgleichung

iodine

(dibenzofuran-3-yl)-diphenyl-phosphine oxide

HCl

lithium diisopropylamide

→

(4-Iodo-dibenzofuran-3-yl)-diphenylphosphineoxide

Lösungsmittel

THF

THF

THF n-heptane

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONis added
2. 2
   Waschenthe solution is washed with sodium thiosulphate solution, water and saturated NaCl solution
3. 3
   Trocknendried with MgSO4
4. 4
   Einengenconcentrated

Vorschrift

9.8 g of (dibenzofuran-3-yl)-diphenyl-phosphine oxide in 100 ml of THF are admixed with 13.3 ml of a 2M solution of lithium diisopropylamide in THF/n-heptane and stirred for a further 10 minutes at -78° C. A solution of 7.9 g of iodine in 30 ml of THF is added at -76° C. Subsequently the mixture is hydrolyzed with 2N HCl, ethyl acetate is added, the solution is washed with sodium thiosulphate solution, water and saturated NaCl solution, dried with MgSO4 and concentrated. 12.7 g (98% of theoretical) of crude product remain.

Quelle