Water → HCID 57815505, Verbindung

HRID 385603

Reaktionsgleichung

Reaktionsgleichung von HRID 385603
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([C:11]([F:14])([F:13])[F:12])=[CH:4][N:3]=1.[OH-].[Na+].O.C(OCC)(=O)C.[CH:24]([C:36]([O:38][CH2:39][CH3:40])=[O:37])([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27]>O1CCCC1>[N+:8]([C:7]1[C:2]([C:24]([C:36]([O:38][CH2:39][CH3:40])=[O:37])([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=[N:3][CH:4]=[C:5]([C:11]([F:14])([F:13])[F:12])[CH:6]=1)([O-:10])=[O:9]

Komponenten

7

Edukt 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 81961Triethyl ethane-1,1,2-tricarboxylateHCID 47369502-Chloro-3-nitro-5-(trifluoromethyl)pyridine

Produkt 1

HCID 57815505HCID 57815505, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 1.8 g of 2-chloro-3-nitro-5-(trifluoromethyl)pyridine in 8 mL of tetrahydrofuran, 2.0 mL of triethyl 1,1,2-ethanetricarboxylate and 0.63 g of 60% sodium hydroxide were added under cooling with ice, and the mixture was stirred at room temperature for 2 hours. Thereto were added water and ethyl acetate, the organic layer was separated, and washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 3.5 g of triethyl 1-(3-nitro-5-(trifluoromethyl)pyridin-2-yl)ethane-1,1,2-tricarboxylate as a brown oily substance.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. customthe organic layer was separated
  3. washwashed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7519d7673304481c9dfabb6e0cbb7e19
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08367831B2

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