Benzene → 1-Phenylcyclohexylperoxy neodecanoate

HRID 1461587

Reaktionsgleichung

Reaktionsgleichung von HRID 1461587
[OH-:1].[K+].[C:3]1([C:9]2([O:15][OH:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C1C=CC=CC=1.[C:23](Cl)(=[O:33])[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([CH3:32])([CH3:31])[CH3:30]>O>[C:23]([O:33][O:16][O:15][C:9]1([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)(=[O:1])[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([CH3:32])([CH3:31])[CH3:30]

Komponenten

6

Edukt 4

HCID 241BenzeneHCID 14797Potassium HydroxideHCID 94502Neodecanoyl chlorideHCID 185715Hydroperoxide, phenylcyclohexyl-

Produkt 1

HCID 199810531-Phenylcyclohexylperoxy neodecanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

In a four-necked flask of 200 ml provided with a stirrer was charged 33.7 g of an aqueous solution of 30% potassium hydroxide, to which was added a mixture of 22.1 g of 95% 1-phenylcyclohexyl hydroperoxide and 30 g of benzene while the liquid temperature was maintained at 10° C. with stirring. Furthermore, 19.1 g of neodecanoyl chloride was added dropwise over 7 minutes while the liquid temperature was maintained at 15° C. with stirring. After the liquid temperature was raised to 25° C. and the stirring was continued for 2 hours, 40 g of cold water was added and further the stirring was made for 5 minutes. The water phase was separated and washed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times. The solution was dried on magnesium sulfate anhydride and benzene was removed off under vacuum to obtain 24.0 g of a desired compound as a light yellow liquid. This compound had an active oxygen amount of 4.20%, a purity of 91% through calculation and a yield of 63 mol %.

Aufarbeitung

  1. customIn a four-necked flask of 200 ml provided with a stirrer
  2. additionto which was added
  3. temperaturewas maintained at 15° C.
  4. stirringwith stirring
  5. temperatureAfter the liquid temperature was raised to 25° C.
  6. waitfurther the stirring was made for 5 minutes
  7. customThe water phase was separated
  8. washwashed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times
  9. dry with materialThe solution was dried on magnesium sulfate anhydride and benzene
  10. customwas removed off under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-5a22fc10ee5b40fb927d43002cfa8982
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05075495

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