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Potassium Carbonate → Ethyl 2-ethyl-4-hydroxy-1-benzofuran-6-carboxylate

HRID 1177262
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1177262
C([O:4][C:5]1[C:10]2[CH:11]=[C:12]([CH2:14][CH3:15])[O:13][C:9]=2[CH:8]=[C:7]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:6]=1)(=O)C.C([O-])([O-])=O.[K+].[K+]>C(O)C>[CH2:14]([C:12]1[O:13][C:9]2[CH:8]=[C:7]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:6]=[C:5]([OH:4])[C:10]=2[CH:11]=1)[CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 59559992Ethyl 4-(acetyloxy)-2-ethyl-1-benzofuran-6-carboxylate

Produkt 1

HCID 59560005Ethyl 2-ethyl-4-hydroxy-1-benzofuran-6-carboxylateAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A suspension of ethyl 4-(acetyloxy)-2-ethyl-1-benzofuran-6-carboxylate (8.0 g, 29.0 mmol) and K2CO3 (4.81 g, 34.8 mmol) in ethanol (80 mL) was refluxed for 24 hours. TLC (petroleum ether/EtOAc 4:1) showed complete consumption of the acetate. The solvent was removed under reduced pressure and the residue was poured into water (30 mL). The aqueous phase was acidified to pH˜2 with 10% aqueous HCl (50 mL) and extracted with EtOAc (100 mL×2). The organic layer was dried over Na2SO4 and concentrated. The residue was purified by column chromatography on silica gel eluted with petroleum ether/EtOAc (40:1) to afford the desired compound (6.0 g, 88%) as a yellow solid. 1H NMR (400 MHz, CDCl3): δ 7.87 (s, 1H), 7.45 (s, 1H), 6.46 (s, 1H), 6.36 (s, 1H), 4.34-4.27 (q, 2H), 2.77-2.71 (q, 2H), 1.40-1.31 (t, 3H), 1.31-1.21 (t, 3H).

Aufarbeitung

  1. temperaturewas refluxed for 24 hours
  2. customconsumption of the acetate
  3. customThe solvent was removed under reduced pressure
  4. additionthe residue was poured into water (30 mL)
  5. extractionextracted with EtOAc (100 mL×2)
  6. dry with materialThe organic layer was dried over Na2SO4
  7. concentrationconcentrated
  8. customThe residue was purified by column chromatography on silica gel
  9. washeluted with petroleum ether/EtOAc (40:1)

Quellen und Nachweise

ORD-Eintrag
ord-093fe5d4cd864c1192b85fdf0b9124d5
Quelldatensatz
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07842713B2

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