Potassium Iodide → Triethyl 2-[4-(trifluoromethoxy)phenyl]ethane-1,1,1-tricarboxylate

HRID 1256884

Reaktionsgleichung

Reaktionsgleichung von HRID 1256884
[CH:1]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:2]([O:4][CH2:5][CH3:6])=[O:3].[F:17][C:18]([F:29])([F:28])[O:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24]Br)=[CH:22][CH:21]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O.C(OCC)(=O)C>[F:17][C:18]([F:28])([F:29])[O:19][C:20]1[CH:21]=[CH:22][C:23]([CH2:24][C:1]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:2]([O:4][CH2:5][CH3:6])=[O:3])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:26][CH:27]=1

Komponenten

8

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 80471Triethyl methanetricarboxylateHCID 1427851-(Bromomethyl)-4-(trifluoromethoxy)benzene

Produkt 1

HCID 68511908Triethyl 2-[4-(trifluoromethoxy)phenyl]ethane-1,1,1-tricarboxylateAusbeute 100,1 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of triethyl methanetricarboxylate (4.55 g) in DMF (40 mL) were added 4-(trifluoromethoxy)benzyl bromide (5.00 g), potassium iodide in catalytic amount and potassium carbonate (4.07 g), and the mixture was stirred at room temperature for 3 hr. Ethyl acetate (200 mL) and water (100 mL) were added to extract the reaction mixture. The extract was washed sequentially with water and brine, and concentrated under reduced pressure to give the title compound (7.97 g) as an oil.

Aufarbeitung

  1. extractionto extract the reaction mixture
  2. washThe extract was washed sequentially with water and brine
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f801f66264d84429acaf4c1228a48aaa
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461209B2

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