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Diisobutylaluminumhydride → HCID 67491360, Verbindung

HRID 880882
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 880882
[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11](OCC)=[O:12].[H-].C([Al+]CC(C)C)C(C)C>C1COCC1>[Br:1][C:2]1[N:6]([C:7]([CH3:8])([CH3:9])[CH3:10])[N:5]=[CH:4][C:3]=1[CH2:11][OH:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21225700DiisobutylaluminumhydrideHCID 53429364Ethyl 5-bromo-1-tert-butyl-1H-pyrazole-4-carboxylate

Produkt 1

HCID 67491360HCID 67491360, VerbindungAusbeute 79,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

A solution of ethyl 5-bromo-1-tert-butyl-1H-pyrazole-4-carboxylate (685 mg, 2.49 mmol) in THF (20 mL) was cooled to −78° C. and treated with diisobutylaluminum hydride (7.47 mL, 7.47 mmol, 1 M THF), dropwise. The mixture was stirred at −78° C. for 30 minutes and then warmed to room temperature for 18 hours. The mixture was quenched with ethyl acetate 10 mL) and stirred 15 minutes. The mixture was then treated with saturated aqueous Rochelle's salt (25 mL) and stirred 1 hour at room temperature. The mixture was diluted with ethyl acetate (100 mL) and washed with water (100 mL). The organic layer was dried over sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography (10-80% ethyl acetate/heptane gradient, 25 g silica gel) to yield 460 mg of (5-bromo-1-tert-butyl-1H-pyrazol-4-yl)methanol as a clear oil. +APCI (M+H) 233.1, (M+2+H) 235.1; 1H NMR (400 MHz, CDCl3, δ): 7.51 (s, 1H), 4.53 (d, 2H), 1.74 (s, 9H), 1.55 (t, J=5.8 Hz, 1H).

Aufarbeitung

  1. temperaturewarmed to room temperature for 18 hours
  2. customThe mixture was quenched with ethyl acetate 10 mL) and
  3. stirringstirred 15 minutes
  4. additionThe mixture was then treated with saturated aqueous Rochelle's salt (25 mL)
  5. stirringstirred 1 hour at room temperature
  6. additionThe mixture was diluted with ethyl acetate (100 mL)
  7. washwashed with water (100 mL)
  8. dry with materialThe organic layer was dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe residue was purified by flash chromatography (10-80% ethyl acetate/heptane gradient, 25 g silica gel)

Quellen und Nachweise

ORD-Eintrag
ord-e4ddd368029545d6843770d30700a150
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08993586B2

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