Potassium Carbonate → HCID 19525517, Verbindung

HRID 58054

Reaktionsgleichung

Reaktionsgleichung von HRID 58054
[Br:1][C:2]1[C:3]([CH3:8])=[N:4][NH:5][C:6]=1[CH3:7].Br[CH2:10][C:11]([NH:13][CH:14]([CH3:16])[CH3:15])=[O:12].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[Br:1][C:2]1[C:3]([CH3:8])=[N:4][N:5]([CH2:10][C:11]([NH:13][CH:14]([CH3:16])[CH3:15])=[O:12])[C:6]=1[CH3:7]

Komponenten

5

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a 4 mL vial equipped with a magnetic stir bar were added 4-bromo-3,5-dimethyl-1H-pyrazole (50 mg, 0.286 mmol), 2-bromo-N-isopropylacetamide (51.4 mg, 0.286 mmol), K2CO3 (118 mg, 0.857 mmol), and acetonitrile (2 mL). The contents of the vial were stirred to give a white suspension. The vial was heated in a sand bath to 70° C. for 24 hours. The reaction mixture was subsequently partitioned between water (10 mL) and ethyl acetate (15 mL). The layers were separated, and the aqueous layer was back-extracted with ethyl acetate (15 mL). The combined organic layers were concentrated to give the title compound as a white solid, which was used without further purification (80 mg).

Aufarbeitung

  1. customTo a 4 mL vial equipped with a magnetic stir bar
  2. customto give a white suspension
  3. customThe reaction mixture was subsequently partitioned between water (10 mL) and ethyl acetate (15 mL)
  4. customThe layers were separated
  5. extractionthe aqueous layer was back-extracted with ethyl acetate (15 mL)
  6. concentrationThe combined organic layers were concentrated

Quellen und Nachweise

ORD-Eintrag
ord-9b7a6a77cab942a590f5687551911879
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434743B2

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