Sodium Carbonate → 4-Bromo-1-(1,1-dimethylethyl)-1H-pyrazole

HRID 57846Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 57846
C([O-])([O-])=O.[Na+].[Na+].[C:7]([N:11]1[CH:15]=[CH:14][CH:13]=[N:12]1)([CH3:10])([CH3:9])[CH3:8].[Br:16]Br>C(Cl)Cl>[Br:16][C:14]1[CH:13]=[N:12][N:11]([C:7]([CH3:10])([CH3:9])[CH3:8])[CH:15]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 24408BromineHCID 134698151-tert-Butyl-1H-pyrazole

Produkt 1

HCID 532168984-Bromo-1-(1,1-dimethylethyl)-1H-pyrazoleAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a suspension of Na2CO3 (3.6 g, 33.9 mmol) in CH2Cl2 (30 mL) was added 1-tert-butyl-1H-pyrazole (2.1 g, 17 mmol) and Br2 (0.9 mL). The mixture was stirred at room temperature overnight. The formed solid was removed by filtration and the filter cake was washed with CH2Cl2 (30 mL). The filtrates were washed with water (20 mL) and brine (20 mL), dried (MgSO4), and concentrated under reduced pressure to afford crude 4-bromo-1-tert-butyl-1H-pyrazole (2.9 g, 85%), which was used in next step without further purification. MS (ESI) m/z: 203 [M+H]+.

Aufarbeitung

  1. customThe formed solid was removed by filtration
  2. washthe filter cake was washed with CH2Cl2 (30 mL)
  3. washThe filtrates were washed with water (20 mL) and brine (20 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a7ee0fd5430a4c08954959ed1e84585a
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434725B2

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