Reaktion #2494

Reaktionsgleichung

4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide

lithium aluminum hydride

→

2-diphenylphosphinomethyl-2'-methyl-1,1'-binaphthyl

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction solution is heated
2. 2
   FiltrationUnreacted lithium aluminum hydride is subsequently filtered off
3. 3
   ExtraktionThe organic phase is extracted with 20 ml of 1N sodium hydroxide solution and subsequently with 20 ml portions of water until the aqueous phase
4. 4
   TrocknenThe organic phase is dried over sodium sulfate
5. 5
   Sonstigeis drawn off at 12 torr/40° C
6. 6
   Sonstigecrystallized

Vorschrift

4 g (7.3 mmol) of 4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide are suspended under a protective gas in 70 ml of absolute toluene. 500 mg (14.3 mmol) of lithium aluminum hydride are added to this suspension and the reaction solution is heated to boiling for 5 hours. Unreacted lithium aluminum hydride is subsequently filtered off. The organic phase is extracted with 20 ml of 1N sodium hydroxide solution and subsequently with 20 ml portions of water until the aqueous phase has a pH of from 6 to 7. The organic phase is dried over sodium sulfate and the toluene is drawn off at 12 torr/40° C. The wax-like residue is admixed with 15 ml of oxygen-free isopropanol, boiled and crystallized.

Quelle