Sodium Iodide → Ethyl 3-Hydroxybutyrate

HRID 327865

Reaktionsgleichung

Reaktionsgleichung von HRID 327865
[Na+].[I-].[C:3]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:4][C:5]([CH3:7])=[O:6].[H][H]>O>[OH:6][CH:5]([CH3:7])[CH2:4][C:3]([O:9][CH2:10][CH3:11])=[O:8]

Komponenten

5

Edukt 3

HCID 5238Sodium IodideHCID 8868Ethyl AcetoacetateHCID 178418361HCID 178418361, Verbindung3×

Produkt 1

HCID 62572Ethyl 3-HydroxybutyrateAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

Under a nitrogen gas atmosphere, 0.0096 g (7.3×10-6 mol) of [RuI(p-Cymene)((+)-SO3Na-BINAP)]I, 0.1164 g (7.8×10-4 mol) of NaI, 1 ml (7.5×10-3 mol) of ethyl acetoacetate, and 1.5 ml of water were charged in a 100 milli-liter autoclave. After displacing the inside atmosphere of the autoclave with a hydrogen gas, the autoclave was pressed at a hydrogen pressure of 50 kg/cm2 and the mixture was stirred for 40 hours at 65° C. After the reaction was over, the hydrogen gas was removed, and after added thereto 100 ml of water and 100 ml of ether, the ether extraction was carried out. The ether extract was recovered, dried with anhydrous sodium sulfate, and further ether was distilled off to provide 0.62 g (percent yield 63%) of ethyl 3-hydroxybutyrate. By the analysis of gas chromatography (PEG-HT), the conversion ratio was determined to be 99%.

Aufarbeitung

  1. customwas removed
  2. additionafter added
  3. extraction100 ml of water and 100 ml of ether, the ether extraction
  4. extractionThe ether extract
  5. customwas recovered
  6. dry with materialdried with anhydrous sodium sulfate, and further ether
  7. distillationwas distilled off

Quellen und Nachweise

ORD-Eintrag
ord-5ab3e6632dd54e23a7176b1dc9864c6e
Quelldatensatz
uspto-grants-1993_12
Patentnummer
US05274146

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