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Sodium Hydroxide → 6-[4-({[3-(2,6-Dichlorophenyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoxalinecarboxylic acid

HRID 2423541
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2423541
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:13]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[CH:23]=[C:24]4[C:29](=[CH:30][CH:31]=3)[N:28]=[C:27]([C:32]([O:34]CC)=[O:33])[CH:26]=[N:25]4)=[CH:18][CH:17]=2)=[C:12]([CH:37]([CH3:39])[CH3:38])[O:11][N:10]=1.[OH-].[Na+]>C(O)C.O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:13]([CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]3[CH:23]=[C:24]4[C:29](=[CH:30][CH:31]=3)[N:28]=[C:27]([C:32]([OH:34])=[O:33])[CH:26]=[N:25]4)=[CH:20][CH:21]=2)=[C:12]([CH:37]([CH3:39])[CH3:38])[O:11][N:10]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 59321561HCID 59321561, Verbindung

Produkt 1

HCID 533200776-[4-({[3-(2,6-Dichlorophenyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoxalinecarboxylic acidAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8028Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

To a stirred solution of ethyl 6-[4-({[3-(2,6-dichlorophenyl) -5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoxalinecarboxylate (0.112 g, 0.20 mmol) in ethanol (5 mL) and tetrahydrofuran (5 mL) was added 1 N sodium hydroxide (0.21 mL, 0.21 mmol). The reaction mixture was stirred at room temperature under nitrogen for 3.5 hours. The solvent was removed in vacuo and water (5 mL) was added to the resulting solid. The pH of the aqueous mixture was adjusted to ˜3 (litmus paper) with 1 N HCl. The acidic aqueous mixture was extracted with ethyl acetate. The aqueous phase was separated and extracted a second time with ethyl acetate. The aqueous phase was separated and found to contain product according to thin layer chromatography. The pH of the aqueous phase was adjusted to ˜2 (litmus paper) with 1 N HCl. The acidic aqueous phase was combined with the aforementioned ethyl acetate extracts. The organic phase was separated, washed with water followed by brine, dried over magnesium sulfate, filtered, and the filtrate was concentrated to give a yellow solid which was dried under high vacuum at room temperature to give 0.095 g (89%) of 6-[4-({[3-(2,6-dichlorophenyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoxalinecarboxylic acid. 1H NMR (d6-DMSO, 400 MHz): δ 13.89 (br s, 1H), 9.40 (s, 1H), 8.32 (s, 1H), 8.24 (m, 2H), 7.81 (d, J=9 Hz, 2H), 7.62 (m, 2H), 7.53 (dd, J=9, 7 Hz, 1H), 6.95 (d, J=9 Hz, 2H), 4.89 (s, 2H), 3.47 (septet, J=7 Hz, 1H), 1.33 (d, J=7 Hz, 6H). ESI-LCMS m/z 532 (M−H)−.

Aufarbeitung

  1. customThe solvent was removed in vacuo and water (5 mL)
  2. additionwas added to the resulting solid
  3. extractionThe acidic aqueous mixture was extracted with ethyl acetate
  4. customThe aqueous phase was separated
  5. extractionextracted a second time with ethyl acetate
  6. customThe aqueous phase was separated
  7. customThe organic phase was separated
  8. washwashed with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. concentrationthe filtrate was concentrated
  12. customto give a yellow solid which
  13. customwas dried under high vacuum at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-da081d1141484218a90b9bc7a5493949
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07960552B2

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