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Water → HCID 10398790, Verbindung

HRID 654686
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 654686
O[C:2]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:14]=1[C:13]([OH:15])=[CH:12][CH:11]=[CH:10]2)([CH3:4])[CH3:3].[OH2:16].N1[CH:22]=[CH:21]C=CC=1>C(O)(=O)C>[C:21]([O:15][C:13]1[C:14]2[C:9](=[CH:8][CH:7]=[CH:6][C:5]=2[C:2]([CH3:4])=[CH2:3])[CH:10]=[CH:11][CH:12]=1)(=[O:16])[CH3:22]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 1049PyridineHCID 10262250HCID 10262250, Verbindung

Produkt 1

HCID 10398790HCID 10398790, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

11.3 g of 8-(1-hydroxy-1-methyl-1-ethyl)-1-naphthol was dissolved in 24 ml of pyridine, to which 12 ml of anhydrous acetic acid was added. The solution was raised in temperature to 60° C. and heated for 6 hours under agitation. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resulting organic phase was washed with a 2N hydrochloric acid aqueous solution, water and a saturated saline solution in this order, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The resultant residue was purified by silica gel column chromatography (10% ethyl acetate/hexane) to obtain 3.6 g of the captioned compound as an oily substance.

Aufarbeitung

  1. additionwas added
  2. temperatureheated for 6 hours under agitation
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe resulting organic phase was washed with a 2N hydrochloric acid aqueous solution, water
  5. dry with materiala saturated saline solution in this order, dried with anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resultant residue was purified by silica gel column chromatography (10% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-10504e77714048f58ef71225b6bcbfc3
Quelldatensatz
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05134111

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