Reaktion #310027

Reaktionsgleichung

propylene pentamer

calcium hydride

calcium

phenol

→

pentadecylphenol calcium salt

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 2-liter round bottom flask equipped with a mechanical stirred, Dean Stark trap
2. 2
   Sonstigefitted with a condenser under an atmosphere of dry nitrogen
3. 3
   TemperaturThe reaction was then heated to 100° C. over 50 minutes
4. 4
   Temperaturheated to 200° C. for over 140 minutes
5. 5
   Temperaturheated to 280° C. over 1 hour
6. 6
   workup.WAITheld at 280° C. for 8.5 hours
7. 7
   Temperaturcooled to 230° C.
8. 8
   workup.WAITheld at 230° C. for approximately 14 hours
9. 9
   TemperaturThe reaction was then cooled to 150° C.
10. 10
    Filtrationfiltered through a dry, hot (150° C.) 600 mL Buchner funnel
11. 11
    workup.ADDITIONcontaining a filter bed of Celite
12. 12
    Temperaturmaintained between 110° C. and 120° C. with the aid of a vacuum
13. 13
    Sonstigeto afford a product

Vorschrift

Branched pentadecylphenol calcium salt was prepared from the alkylation of phenol with a branched chain C14-C18 olefin derived primarily from propylene pentamer. To a 2-liter round bottom flask equipped with a mechanical stirred, Dean Stark trap fitted with a condenser under an atmosphere of dry nitrogen was charged with 705 gm (2.32 moles) of a C15 branched alkylphenol followed by 500 gm of Chevron RLOP 100N oil. This mixture was cooled to approximately 13° C. using an ice bath and then 48.8 gm (1.16 moles) of calcium hydride (98% obtained from Aldrich Chemical Company) was added in approximately 10 gram portions with stirring. The reaction was then heated to 100° C. over 50 minutes and then heated to 200° C. for over 140 minutes and held at 200° C. for approximately 18 hours and then heated to 280° C. over 1 hour and held at 280° C. for 8.5 hours and then cooled to 230° C. and held at 230° C. for approximately 14 hours. The reaction was then cooled to 150° C. and filtered through a dry, hot (150° C.) 600 mL Buchner funnel containing a filter bed of Celite and maintained between 110° C. and 120° C. with the aid of a vacuum to afford a product containing 3.51 wt % calcium.

Quelle