Cyanide → HCID 53467828, Verbindung

HRID 2401169Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2401169
Br[C:2]1[C:3]([NH2:18])=[N:4][C:5]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)=[N:6][C:7]=1[N:8]1[CH:12]=[CH:11][CH:10]=[N:9]1.[C-:19]#[N:20].C(OCC)(=O)C>N1C=CC=CC=1>[NH2:18][C:3]1[C:2]([C:19]#[N:20])=[C:7]([N:8]2[CH:12]=[CH:11][CH:10]=[N:9]2)[N:6]=[C:5]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)[N:4]=1

Komponenten

5

Edukt 3

HCID 5975CyanideHCID 8857Ethyl AcetateHCID 534669585-bromo-2,6-di(1H-pyrazol-1-yl)pyrimidin-4-amine

Produkt 1

HCID 53467828HCID 53467828, VerbindungAusbeute 39,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A mixture of 0.2 g (0.65 mmol) of 5-bromo-2,6-di(1H-pyrazol-1-yl)pyrimidin-4-amine and 0.06 g (0.72 mmol) of cupper (I) cyanide in 3 ml of pyridine was irradiated with microwaves at 250° C. for 20 min. After nearly complete conversion to the corresponding carbonitrile as was indicated by TLC, ethyl acetate was added and filtered throw celite. The solution was extracted two times with 10 ml of saturated solution of NaHCO3 and Brine. The organic layer was separated, dried with MgSO4 and concentrated to give 0.065 g (39.6%) of the desired product.

Aufarbeitung

  1. customwas irradiated with microwaves at 250° C. for 20 min
  2. additionwas added
  3. filtrationfiltered
  4. extractionThe solution was extracted two times with 10 ml of saturated solution of NaHCO3 and Brine
  5. customThe organic layer was separated
  6. dry with materialdried with MgSO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8b7352c0616d400a96ca13f3e0890d8c
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08796284B2

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