Water → HCID 12769820, Verbindung

HRID 26687

Reaktionsgleichung

Reaktionsgleichung von HRID 26687
[CH2:1]([CH:3]1[CH:8]([CH3:9])[C:7](=[O:10])[C:6]2[CH:11]=[C:12]([CH:15]([CH3:20])[C:16]([O:18]C)=[O:17])[CH:13]=[CH:14][C:5]=2[O:4]1)[CH3:2].C(=O)(O)[O-].[Na+].O>C(O)C>[CH2:1]([CH:3]1[CH:8]([CH3:9])[C:7](=[O:10])[C:6]2[CH:11]=[C:12]([CH:15]([CH3:20])[C:16]([OH:18])=[O:17])[CH:13]=[CH:14][C:5]=2[O:4]1)[CH3:2]

Komponenten

5

Edukt 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 21322013Methyl 2-[2,3-dihydro-2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate

Produkt 1

HCID 12769820HCID 12769820, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Methyl 2-[2,3-dihydro-2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate (6 g) was dissolved in ethanol (200 ml) and heated to reflux with dilute aqueous sodium bicarbonate solution (50 ml) for eight hours. The reaction mixture was poured into water, acidified and extracted with ether. The combined etheral extracts were washed with water and dried (MgSO4) and concentrated in vacuo affording a mixture of the desired product and starting material which were separated by chromatography on silica gel using dichloromethane/ether mixtures as eluant. The title compound was recrystallised from petroleum ether (bp 40°-60° C.) as a white solid: 1.4 g, mp 114°-115° C.

Aufarbeitung

  1. temperatureheated
  2. extractionextracted with ether
  3. washThe combined etheral extracts were washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customaffording

Quellen und Nachweise

ORD-Eintrag
ord-c6d54deac7e142829d3b2da97761ea92
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04151179

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