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1-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole → 5-(1-methyl-1H-pyrazol-4-yl)-2-naphthoic acid

HRID 59606
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 59606
Br[C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([C:12]([OH:14])=[O:13])=[CH:7]2.[CH3:15][N:16]1[CH:20]=[C:19](B2OC(C)(C)C(C)(C)O2)[CH:18]=[N:17]1>C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:15][N:16]1[CH:20]=[C:19]([C:2]2[CH:11]=[CH:10][CH:9]=[C:8]3[C:3]=2[CH:4]=[CH:5][C:6]([C:12]([OH:14])=[O:13])=[CH:7]3)[CH:18]=[N:17]1
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Komponenten

5

Edukt 2

HCID 27739871-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 149606465-Bromonaphthalene-2-carboxylic acid

Produkt 1

HCID 685128445-(1-methyl-1H-pyrazol-4-yl)-2-naphthoic acidAusbeute 34 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418397HCID 178418397, VerbindungKatalysator
HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

A mixture of 5-bromo-2-naphthoic acid (2.12 g, 8.44 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (1.84 g, 8.86 mmol), and tetrakis(triphenylphosphine)palladium(0) (502 mg, 0.435 mmol) in a 250 mL round bottomed flask was evacuated and purged with nitrogen (in three cycles). Acetonitrile (40 mL) and 2M aqueous sodium carbonate (10 mL) were added to the mixture via syringe, and the mixture was heated under reflux under nitrogen for 22 hours. The reaction mixture was allowed to cool before the addition of 1M aqueous hydrochloric acid (30 mL) and it was then extracted with ethyl acetate (3×50 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated in vacuo to provide a crude product (2.98 g after air drying). This crude material was dissolved in hot ethanol (150 mL) and filtered while hot to remove a yellow impurity (120 mg). The filtrate was concentrated in vacuo and the residue was recrystallised from dichloromethane (30 mL) to provide 5-(1-methyl-1H-pyrazol-4-yl)-2-naphthoic acid as a white solid (724 mg, 34%). A second crop of 5-(1-methyl-1H-pyrazol-4-yl)-2-naphthoic acid (527 mg, 25%) was obtained from the concentrated mother liquors by recrystallisation from dichloromethane (20 mL).

Aufarbeitung

  1. customwas evacuated
  2. custompurged with nitrogen (in three cycles)
  3. additionAcetonitrile (40 mL) and 2M aqueous sodium carbonate (10 mL) were added to the mixture via syringe
  4. temperaturethe mixture was heated
  5. temperatureunder reflux under nitrogen for 22 hours
  6. temperatureto cool before the addition of 1M aqueous hydrochloric acid (30 mL) and it
  7. extractionwas then extracted with ethyl acetate (3×50 mL)
  8. dry with materialThe combined organic layers were dried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customto provide a crude product (2.98 g after air drying)
  12. filtrationfiltered while hot
  13. customto remove a yellow impurity (120 mg)
  14. concentrationThe filtrate was concentrated in vacuo
  15. customthe residue was recrystallised from dichloromethane (30 mL)

Quellen und Nachweise

ORD-Eintrag
ord-e7da42e80ab04e81b347cd39c4d118af
Quelldatensatz
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09440926B2

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