Potassium Hydroxide → HCID 67166457, Verbindung

HRID 552378Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 552378
[CH2:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[C:5]=1[C:6]([O:8]C)=[O:7])[CH:2]=[CH2:3].[OH-].[K+]>C(O)C>[CH2:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[C:5]=1[C:6]([OH:8])=[O:7])[CH:2]=[CH2:3]

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 67166341HCID 67166341, Verbindung

Produkt 1

HCID 67166457HCID 67166457, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of Step 2 intermediate (3.0 g, 15.7 mmol) in ethanol (10 ml) was added 2.0 M potassium hydroxide (4.0 ml) and the mixture was refluxed for 3 h. The mixture was concentrated under reduced pressure and diluted with water. The basic aqueous solution containing the product was washed with diethyl ether (2×25 ml). The aqueous solution was acidified to pH 4.0 with 1N HCl. The solid separated out was filtered and washed with water and dried to give 550 mg of the product as an off-white solid; 1H NMR (δ ppm, CDCl3, 300 MHz): 7.01 (t, J=9.0, 1H); 6.57 (d, J=9.0, 1H); 6.36 (d, J=9.0, 1H); 5.94-5.79 (m, 1H); 5.02-4.90 (m, 2H); 3.46 (d, J=6.0, 2H).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 3 h
  2. concentrationThe mixture was concentrated under reduced pressure
  3. additiondiluted with water
  4. additionThe basic aqueous solution containing the product
  5. washwas washed with diethyl ether (2×25 ml)
  6. customThe solid separated out
  7. filtrationwas filtered
  8. washwashed with water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-011adf86833f48258e5f6aa0bc4bfe44
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07951814B2

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