Ethyl Acetoacetate → HCID 178472877, Verbindung

HRID 75488Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 75488
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[N:10]([O-])=[O:11].[Na+]>C(O)(=O)C.O>[OH:11][N:10]=[C:2]([C:3](=[O:4])[CH3:5])[C:1]([O:7][CH2:8][CH3:9])=[O:6]

Komponenten

5

Edukt 2

HCID 8868Ethyl Acetoacetate2×HCID 23668193Sodium Nitrite

Produkt 1

HCID 178472877HCID 178472877, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a solution of ethyl acetoacetate (compound 7, 30 g, 0.23 mol) in acetic acid (35 mL) was added slowly sodium nitrite (18.0 g, 0.25 mol) in cold water (40 mL) at −10° C. The reaction mixture was stirred for 1 hr, then added cold water (120 mL) and stirred for 3 hrs. The mixture was extracted with diethyl ether (300 mL). The organic layer was washed with saturated NaHCO3 (400 mL×2), then dried over anhydrous MgSO4, filtered and concentrated in vacuo. The obtained product (21.46 g, white solid) was used for the next step without purification.

Aufarbeitung

  1. stirringstirred for 3 hrs
  2. extractionThe mixture was extracted with diethyl ether (300 mL)
  3. washThe organic layer was washed with saturated NaHCO3 (400 mL×2)
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe obtained product (21.46 g, white solid) was used for the next step without purification

Quellen und Nachweise

ORD-Eintrag
ord-38b8e18b3cb54831ab47c0f5dcaddc64
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835436B2

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