Hydrochloric Acid → HCID 57983386, Verbindung

HRID 2078325Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2078325
Cl.[Br:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH3:21])([CH3:20])[C:8](=[O:19])[C:9](C(OCC)=O)=[C:10]2[OH:13])=[CH:5][CH:4]=1>C(O)(C(F)(F)F)=O>[Br:2][C:3]1[CH:12]=[C:11]2[C:6](=[CH:5][CH:4]=1)[C:7]([CH3:21])([CH3:20])[C:8](=[O:19])[CH:9]=[C:10]2[OH:13]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 67099861HCID 67099861, Verbindung

Produkt 1

HCID 57983386HCID 57983386, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Concentrated aqueous HCl (36.5-37.5%, 10 mL) was added to a solution of ethyl 7-bromo-1-hydroxy-4,4-dimethyl-3-oxo-3,4-dihydronaphthalene-2-carboxylate (1.40 g, 4 mmol) in TFA (10 mL). The mixture was heated to 80° C. for 18 hours. The solvent was then removed under reduced pressure, and the residue was rinsed with water and diethyl ether. The remaining solids were dried in vacuo at 50° C. to afford the title compound in 70% yield. 1H-NMR (300 MHz, DMSO-d6) δ ppm 7.98 (1H, d, J=1.9 Hz), 7.75 (1H, dd, J=2.0, 8.5 Hz), 7.67 (1H, br. d, J˜8.0 Hz), 5.64 (1H, s), 2.51 (6H, m). MS (m/z not observed).

Aufarbeitung

  1. customThe solvent was then removed under reduced pressure
  2. washthe residue was rinsed with water and diethyl ether
  3. customThe remaining solids were dried in vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-797be1b8f6c4414da9513405686e9bdf
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928139B2

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