Reaktion #157117

Reaktionsgleichung

5-bromo-2-(2,6-difluorophenyl)pyrimidine-4-carboxylic acid

ammonium hydroxide

→

5-amino-2-(2,6-difluorophenyl)pyrimidine-4-carboxylic acid

Lösungsmittel

dry ice

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenunsealed and concentrated in vacuo
2. 2
   workup.ADDITIONTo the resulting solids was added 1.0 N HCl
3. 3
   Extraktionthe mixture was extracted with EtOAc
4. 4
   WaschenCombined organic extracts were washed once with brine
5. 5
   Trocknendried over anhydrous Na2SO4
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated in vacuo

Vorschrift

CuSO4 (0.1 eq) was added to a mixture of 5-bromo-2-(2,6-difluorophenyl)pyrimidine-4-carboxylic acid (1 eq) and 28% aqueous ammonium hydroxide solution in a microwave reaction vessel. The reaction mixture was heated in a microwave reactor at 110° C. for 25 min. The reaction vessel was cooled in dry ice for 30 min then unsealed and concentrated in vacuo. To the resulting solids was added 1.0 N HCl and the mixture was extracted with EtOAc. Combined organic extracts were washed once with brine, then dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 5-amino-2-(2,6-difluorophenyl)pyrimidine-4-carboxylic acid. The crude product was used for the next step without further purification. LC/MS (m/z): 252.0 (MH+). LC: Rt: 2.043 min.

Quelle