Lithium Hydroxide → HCID 66857134, Verbindung

HRID 1042503Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1042503
C([O:3][C:4](=[O:21])[C:5]([CH3:20])=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][C:8]=1[CH2:17][CH2:18][CH3:19])C.[Li+].[OH-]>C1COCC1.O>[CH3:20][C:5](=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([F:14])([F:15])[F:16])=[CH:9][C:8]=1[CH2:17][CH2:18][CH3:19])[C:4]([OH:21])=[O:3]

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 66856173HCID 66856173, Verbindung

Produkt 1

HCID 66857134HCID 66857134, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a suspension of 2-methyl-3-(2-propyl-4-trifluoromethyl-phenyl)-acrylic acid ethyl ester (68 mg, 0.23 mmol) in THF (1 mL) was added a solution of 1N-LiOH (10 ml), and the mixture was stirred for 3 hours at room temperature. The resulting residue was dissolved in H2O and then washed three times with EtOAc, acidified with 1N HCl to pH 1-2. The solution was extracted three times with methylene chloride and then dried over anhydrous MgSO4 and concentrated in vacuo to give the title compound (60 mg, 96%).

Aufarbeitung

  1. washwashed three times with EtOAc
  2. extractionThe solution was extracted three times with methylene chloride
  3. dry with materialdried over anhydrous MgSO4
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-14c1c645b90048b38b2b77dd907ebbae
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08557872B2

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