Lithium hydroxide, monohydrate → 2-(5-(Trifluoromethyl)pyridin-2-yl)benzoic acid

HRID 841775

Reaktionsgleichung

Reaktionsgleichung von HRID 841775
C([O:4][C:5](=[O:22])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][N:13]=1)(C)C.O.[OH-].[Li+]>O1CCCC1CO.O>[F:20][C:18]([F:19])([F:21])[C:15]1[CH:16]=[CH:17][C:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]([OH:22])=[O:4])=[N:13][CH:14]=1

Komponenten

4

Versuchsvorschrift

2-(5-Trifluoromethyl-pyridin-2-yl)-benzoic acid isopropyl ester was dissolved in 10 ml of a 3:1:1 mixture of tetrahydrofuran-methanol-water, and lithium hydroxide monohydrate (161 mg, 3.84 mmol) was added. After stirring for 3 h at room temperature, the volatiles were removed under vacuum and 5 ml of water were added to the mixture, which was brought to pH 6 with 1N HCl. The resulting slurry was extracted with ethyl acetate, the combined organic layers were dried (magnesium sulfate), filtered and concentrated under vacuum to provide the title compound.

Aufarbeitung

  1. additionwas added
  2. customthe volatiles were removed under vacuum and 5 ml of water
  3. additionwere added to the mixture, which
  4. extractionThe resulting slurry was extracted with ethyl acetate
  5. dry with materialthe combined organic layers were dried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ba7b74c984b54a368ce98a401e2c202e
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06369075B1

Verknüpfte Notizen

Wird geladen…