Reaktion #166149

Reaktionsgleichung

(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine

2,6-dimethyl-2,5-heptadien-4-one

→

2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-one

Ausbeute 76.1%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe vessel was purged with argon gas
2. 2
   Sonstigeimmersed in an oil bath at 170° C. with magnetic stirring
3. 3
   SonstigeThe flask was sealed with a Teflon stopcock
4. 4
   SonstigeThe flask was removed from the oil bath after 14 h
5. 5
   workup.ADDITIONAnhydrous ethanol (70 mL) was added to the unpurified solids
6. 6
   TemperaturThe slurry was warmed to 80° C.
7. 7
   workup.WAITheld for an hour
8. 8
   Temperaturcooled to room temperature
9. 9
   SonstigeThe product was isolated by filtration, washes with ethanol
10. 10
    Sonstigedried in vacuo

Vorschrift

A flask was charged with 10.8 g of (2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (66% potent, 7.13 g, 22.8 mmol, 1.0 equiv) and 6.6 g of 2,6-dimethyl-2,5-heptadien-4-one (47.7 mmol, 2.1 equiv). The vessel was purged with argon gas and immersed in an oil bath at 170° C. with magnetic stirring. The flask was sealed with a Teflon stopcock and the reaction was allowed to proceed under a static argon atmosphere. The flask was removed from the oil bath after 14 h and the contents allowed to cool to room temperature under argon gas. Anhydrous ethanol (70 mL) was added to the unpurified solids and the solids were broken up manually. The slurry was warmed to 80° C., held for an hour, and cooled to room temperature. The product was isolated by filtration, washes with ethanol and dried in vacuo to give 7.82 g of 2,2,6,6-tetramethyl-1-(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphinan-4-one (98 area % by HPLC, 74% yield).

Quelle