Ethylene Oxide → 2-Naphthol Ether

HRID 1351042

Reaktionsgleichung

Reaktionsgleichung von HRID 1351042
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[OH:11].[CH2:12]1[O:15][CH:13]1[CH3:14].[CH2:16]1OC1.C1OC1C.C1OC1>C1(C)C=CC=CC=1>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[OH:11].[CH3:14][CH2:13][O:15][CH2:12][CH3:16]

Komponenten

6

Edukt 4

HCID 6354Ethylene OxideHCID 6378Propylene OxideHCID 86632-NaphtholHCID 24751Crl-8131

Produkt 1

HCID 197425842-Naphthol Ether

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

To a clean, dry stirred tank pressure vessel with nitrogen inlet is charged 952.71 g (6.61 moles) of 2-Naphthol and 1445 mLs of Toluene. The vessel is purged with nitrogen and a catalytic amount (4.96 g) of BF3/Etherate Solution is charged. The temperature is raised to 110° C. and a mixture of 1919.03 g (33.04 moles) of Propylene Oxide and 873.28 g (19.82 moles) of Ethylene Oxide is added at a constant rate to keep the pressure inside the vessel below 50 psig. After all Propylene Oxide/Ethylene Oxide is added, the reaction mixture is allowed to react for an additional 3 hours after which the temperature is raised to 150° C. and the toluene is distilled off under nitrogen sparge. After the distillation of Toluene, the temperature is cooled to 110° C. and vacuum is applied for 1 hour.

Aufarbeitung

  1. customTo a clean, dry
  2. customThe vessel is purged with nitrogen
  3. additiona catalytic amount (4.96 g) of BF3/Etherate Solution is charged
  4. additionis added at a constant rate
  5. customto react for an additional 3 hours after which the temperature
  6. temperatureis raised to 150° C.
  7. distillationthe toluene is distilled off under nitrogen
  8. customsparge
  9. distillationAfter the distillation of Toluene
  10. temperaturethe temperature is cooled to 110° C.

Quellen und Nachweise

ORD-Eintrag
ord-d25ef7225f0d42b3a4b153acd568a894
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07217424B2

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