Potassium Iodide → 2,6-Diphenylphenoxyethanol

HRID 539432

Reaktionsgleichung

Reaktionsgleichung von HRID 539432
[C:1](OC1C=CC(C(C2C=CC(OC(=O)C=C)=CC=2)(C2C=CC(OC(=O)C=C)=CC=2)C)=CC=1)(=[O:4])[CH:2]=C.[C:36]1([C:42]2[CH:47]=[CH:46][CH:45]=[C:44]([C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)[C:43]=2[OH:54])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.C1(=O)OCCO1.[I-].[K+].CN(C)C=O>C(OCC)(=O)C>[C:48]1([C:44]2[CH:45]=[CH:46][CH:47]=[C:42]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:43]=2[O:54][CH:1]([OH:4])[CH3:2])[CH:49]=[CH:50][CH:51]=[CH:52][CH:53]=1

Komponenten

7

Edukt 5

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 7303Ethylene carbonateHCID 755122,6-DiphenylphenolHCID 11568972HCID 11568972, Verbindung

Produkt 1

HCID 689761212,6-Diphenylphenoxyethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a 50 ml 1 neck round bottom was added 2,6-diphenylphenol (10 g, 1 eq), ethylene carbonate (3.9 g, 1.1 eq), potassium iodide (0.07 g, 0.01 eq), dimethylformamide (1 g, 0.3 eq) and heated to 150 C. After 4 hours the reaction was cooled to 40 C, added 30 ml ethyl acetate and washed 2 times with 20 ml sodium chloride brine, 3 times with 20 ml DI water and again with 20 ml brine. The ethyl acetate was dried with (1 g) magnesium sulfate, filtered and concentrated invacuo to recover an off-white solid. Mp 77-78

Aufarbeitung

  1. temperatureheated to 150 C
  2. temperatureAfter 4 hours the reaction was cooled to 40 C
  3. washwashed 2 times with 20 ml sodium chloride brine, 3 times with 20 ml DI water
  4. dry with materialThe ethyl acetate was dried with (1 g) magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated invacuo
  7. customto recover an off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-ed67fd6e96f74bf291907cf63504f9d2
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08871315B2

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