Acetic Acid → HCID 68217647, Verbindung

HRID 1661055Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1661055
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C:7](=O)[CH2:6][CH2:5]2.[C:14]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])#[N:15].CC(O)=O.C([O-])(=O)C.[NH4+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])/[C:7](=[C:16](\[C:14]#[N:15])/[C:17]([O:19][CH2:20][CH3:21])=[O:18])/[CH2:6][CH2:5]2

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 7764Ethyl cyanoacetateHCID 517165Ammonium AcetateHCID 109214765-Chloro-6-methoxy-1-indanone

Produkt 1

HCID 68217647HCID 68217647, VerbindungAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To the solution of 5-chloro-6-methoxy-2,3-dihydro-1H-inden-1-one (Prep15, 12 g, 61.2 mmol) in toluene (240 ml) was added ethyl cyanoacetate (8.3 g, 73.46 mmol), AcOH (48 ml, 0.8 mol) and ammonium acetate (12 g, 0.16 mol). The mixture was stirred for 12 hours at 120° C., checked by TLC, concentrated, filtered and washed with water and ethanol twice and purified by FC to afford 11 g of title compound (y=62%).

Aufarbeitung

  1. concentrationconcentrated
  2. filtrationfiltered
  3. washwashed with water and ethanol twice
  4. custompurified by FC

Quellen und Nachweise

ORD-Eintrag
ord-6d5a1f520e3e4784be214b4193ac042d
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08030322B2

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