Hydrochloric Acid → 2-sec-Butylphenol
Reaktionsgleichung
[CH:1]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7](C(CC)C)[C:6]=1[OH:15])([CH2:3][CH3:4])[CH3:2].CCC=C.Cl>>[CH:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[OH:15])([CH2:3][CH3:4])[CH3:2]Komponenten
Reaktionsbedingungen
- Temperatur
- 275 °C
Versuchsvorschrift
In the reaction vessel of Example 1 place 190 parts of phenol and 2.4 parts of granular aluminum. Flush with nitrogen and heat to 180°C. to form aluminum phenoxide. Cool and vent. Add 206 parts of 2,6-di-sec-butylphenol and again seal the vessel. Heat to 275°C. and stir at this temperature for 2 hours. Then pressurized with butene-1 to 1000 psig and stir the reaction mixture under these conditions for an additional 4 hours. Cool and discharge the reaction mixture into a dilute aqueous hydrochloric acid solution to hydrolyze the catalyst. Wash with water until neutral and then distill the reaction mixture to recover o-sec-butylphenol. Residual 2,6-di-sec-butylphenol remaining is recycled to a subsequent reaction carried out in the same manner as the foregoing. The net result is that the 2,6-di-sec-butylphenol formed in each reaction is consumed in a subsequent reaction as the donor phenol forming o-sec-butylphenol, thus, avoiding accumulation of 2,6-di-sec-butylphenol and giving higher yields of o-sec-butylphenol.
Aufarbeitung
- temperatureCool
- customagain seal the vessel
- stirringstir the reaction mixture under these conditions for an additional 4 hours
- temperatureCool
- washWash with water until neutral and
- distillationthen distill the reaction mixture
- customto recover o-sec-butylphenol
- customResidual 2,6-di-sec-butylphenol remaining is recycled to a subsequent reaction
- customThe net result
- customformed in each reaction
- customis consumed in a subsequent reaction as the donor phenol
Quellen und Nachweise
- ORD-Eintrag
- ord-0b4436dd2c2542b4bcb63dd110dc4851
- Quelldatensatz
- uspto-grants-1976_01
- Patentnummer
- US03933927
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