Propionic Acid → 2-(5,6-Dimethoxy-3,3-dimethyl-1-indanylidene)-4,4-dimethyl-3-oxo-pentanonitrile

HRID 1271791Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1271791
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=O)[CH2:7][C:6]2([CH3:16])[CH3:15].[C:17]([CH2:23][C:24]#[N:25])(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19].C(O)(=O)CC.C([O-])(=O)C.[NH4+]>C1(C)C(C)=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=[C:23]([C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[C:24]#[N:25])[CH2:7][C:6]2([CH3:16])[CH3:15]

Komponenten

6

Edukt 4

HCID 1032Propionic AcidHCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 138129z1-Indanone, 5,6-dimethoxy-3,3-dimethyl-HCID 517165Ammonium Acetate

Produkt 1

HCID 694270512-(5,6-Dimethoxy-3,3-dimethyl-1-indanylidene)-4,4-dimethyl-3-oxo-pentanonitrileAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

44 g (0.2 mol) of 5,6-dimethoxy-3,3-dimethyl-1-indanone, 25 g (0.2 mol) of pivaloylacetonitrile, 32 g of propionic acid and 17 g of ammonium acetate are mixed in 80 g of xylene and heated at 120° C. for 7 hours. After the system has been cooled to room temperature and the organic phase has been washed, the xylene is distilled off, and the crude product which remains is recrystallized in methanol. Yield: 50% theory; E1/1730 (λmax 373 nm).

Aufarbeitung

  1. temperatureAfter the system has been cooled to room temperature
  2. washthe organic phase has been washed
  3. distillationthe xylene is distilled off
  4. customthe crude product which remains is recrystallized in methanol

Quellen und Nachweise

ORD-Eintrag
ord-eb3f1430fc584b66bb8f417be2d4e2de
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07208142B2

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