Potassium Carbonate → HCID 71087246, Verbindung

HRID 571882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 571882
[F:1][C:2]([F:20])([F:19])[C:3]1[N:8]=[C:7]([N:9]2[CH:13]=[C:12]([C:14]([O:16]CC)=[O:15])[CH:11]=[N:10]2)[CH:6]=[N:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[F:20][C:2]([F:1])([F:19])[C:3]1[N:8]=[C:7]([N:9]2[CH:13]=[C:12]([C:14]([OH:16])=[O:15])[CH:11]=[N:10]2)[CH:6]=[N:5][CH:4]=1

Komponenten

5

Edukt 2

HCID 11430Potassium Carbonate2×HCID 71086736HCID 71086736, Verbindung

Produkt 1

HCID 71087246HCID 71087246, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Under N2, ethyl 1-(6-(trifluoromethyl)pyrazin-2-yl)-1H-pyrazole-4-carboxylate (155 mg, 542 μmol, Eq: 1.00) was dissolved in DMF (9.3 ml) and Water (9.3 ml). Potassium carbonate (150 mg, 1.08 mmol, Eq: 2) was added and the RM was stirred at 70° C. overnight. Control with LC-MS: Pr/SM: 74/26. Potassium carbonate (150 mg, 1.08 mmol, Eq: 2) was added and the RM was stirred at 70° C. overnight. Control with LC-MS: SM/Pr:4/96. At RT, the RM was partitioned between 1M K2CO3 and EtOAc; extracted; the water layer was acidified with 1M HCl; extracted with EtOAc; the organic phase was dried over MgSO4; filtered; concentrated in vacuo leading to 132 mg off-white solid.

Aufarbeitung

  1. stirringthe RM was stirred at 70° C. overnight
  2. customAt RT, the RM was partitioned between 1M K2CO3 and EtOAc
  3. extractionextracted
  4. extractionextracted with EtOAc
  5. dry with materialthe organic phase was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e48d97ec530440688a6e5735f50ca842
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029370B2

Notizen zur Reaktion

Wird geladen…