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Lithium hydroxide, monohydrate → 6-Chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylic acid

HRID 253696
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 253696
C[O:2][C:3]([C:5]1[C:13]2[O:12][N:11]=[C:10]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([CH2:21][CH3:22])=[CH:17][CH:16]=3)[C:9]=2[CH:8]=[CH:7][C:6]=1[Cl:23])=[O:4].O[Li].O>O1CCOCC1>[Cl:23][C:6]1[CH:7]=[CH:8][C:9]2[C:10]([NH:14][C:15]3[CH:16]=[CH:17][C:18]([CH2:21][CH3:22])=[CH:19][CH:20]=3)=[N:11][O:12][C:13]=2[C:5]=1[C:3]([OH:4])=[O:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 59805810Methyl-6-chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylate

Produkt 1

HCID 598058146-Chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of methyl-6-chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylate (211 mg, 638 μmol) in dioxane (10.5 ml) was added a 1N aqueous solution of LiOH hydrate (134 mg, 3190 μmol) and the resulting mixture was heated to 50° C. After 1 hr, the solvent was removed in vacuo, the residue was diluted with H2O and acidified to pH2 with 2N HCl. After diluting with EtOAc, the layers were separated and the aqueous layer was extracted with EtOAc (3×). The organics were combined, washed with brine, dried over MgSO4, filtered and concentrated to obtain the title compound as a brown solid, which was used without further purification.

Aufarbeitung

  1. customthe solvent was removed in vacuo
  2. additionthe residue was diluted with H2O
  3. additionAfter diluting with EtOAc
  4. customthe layers were separated
  5. extractionthe aqueous layer was extracted with EtOAc (3×)
  6. washwashed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-6614d84e87124a8687ca5bb0091b0b01
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07872128B2

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