Potassium Carbonate → 2-Amino-3-cyano-5-ethynylpyrazine

HRID 1683678Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1683678
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[N:6][C:5]([C:10]#[C:11][Si](C)(C)C)=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+]>CO>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[N:6][C:5]([C:10]#[CH:11])=[CH:4][N:3]=1

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 153352712-Amino-3-cyano-5-(trimethylsilylethynyl)pyrazine

Produkt 1

HCID 153352732-Amino-3-cyano-5-ethynylpyrazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 1.3 grams (0.006 mole) of 2-amino-3-cyano-5-(trimethylsilylethynyl)pyrazine and 0.9 gram (0.006 mole) of potassium carbonate in 50 mL of methanol is stirred at ambient temperature for one hour. The reaction mixture is then concentrated under reduced pressure to a residue. The residue is taken up in about 75 mL of water, and the solution is extracted with two 200 mL portions of ethyl acetate. The combined extracts are dried with magnesium sulfate and filtered. The filtrate is concentrated under reduced pressure, yielding 2-amino-3-cyano-5-ethynylpyrazine. This reaction is repeated several times.

Aufarbeitung

  1. concentrationThe reaction mixture is then concentrated under reduced pressure to a residue
  2. extractionthe solution is extracted with two 200 mL portions of ethyl acetate
  3. dry with materialThe combined extracts are dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0653129c78bc404bb9ca72d0696e6902
Quelldatensatz
uspto-grants-1997_06
Patentnummer
US05639753

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